Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
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Z racji tego że wielu początkującym chemikom, ćpunom, czy innym osobom które chcą zarobić parę groszy, redukcja fenylonitropropenu amalgamatem aluminium
po prostu nie wychodzi, postanowiłem wyjść z pomocą. Głównym powodem dla którego po zmieszaniu amalgamatu z esencją octową, ipa i p2np nie dzieje się nic
jest brak amalgamatu na powierzchni aluminium. Dzieje się tak, ponieważ folia aluminiowa jest zbyt cienka, i albo jest zjadana podczas amalgowania,
albo wymywamy amalgamat przepłukując go wodą. Można tego uniknąć na dwa sposoby.
1. użyć grubszego źródła aluminium (np. aluminiowe tacki do grilla)
2. redukować i amalgować jednocześnie.
Ja skupię się na metodzie drugiej. Cała reakcja wygląda tak, że do 1l kolby lub słoika wsypujemy:
-pociętą w trójkąty równoramienne folię aluminiową w ilości 8g
-P2NP;fenylonitropropen 5g
-IPA;izopropanol 50ml (do kupienia w sklepach komputerowych, jest używany do czyszczenia)
-esencja octowa (kwas octowy 80%) 50ml (ewentualnie rozcieńczyć lodowaty kwas octowy)
-HgCl2; chlorek rtęci (III) 30mg (ilość możecie dobrać doświadczalnie, lepiej nie dawać więcej jeśli robicie duże ilości ponieważ całość wypierdoli z kolby)
Jeśli jest możliwość zakładamy na kolbę chłodnicę w trybie zwrotnym, czyli pionowo, i odpalamy przepływ wody przez nią, jeśli nie mamy to nie zakładamy.
Po kilku minutach nasza mieszanina zaczyna się nagrzewać, wtedy powinniśmy całość wymieszać ponieważ p2np rozpuszcza sie w ciepłych rozpuszczalnikach.
Gdy p2np się rozpuści, naszą kolbę lub słoik wsadzamy do garnka/wiadra/wanny/kibla/przerębla/rzeki z zimną wodą. Jest to konieczne bo gdy reakcja się rozpędza,
całość zaczyna się mocno nagrzewać, tak że nawet nie będziemy w stanie utrzymać kolby w ręce, poza tym całość może wyjebać poza kolbę.
Zanurzając kolbę lub słoik w wodzie kontrolujemy reakcję, jeśli widzimy, że całość mieści się w naczyniu, wyciągamy je. Po około 10-15 minutach większość
fenylonitropropenu jest już zredukowana jednak my chcąc zwiększyć wydajność naszej reakcji, wsadzamy nasze naczynie reakcyjne (słoik lub kolba) do łaźni wodnej,
czyli do garnka z wodą lub olejem, który kładziemy na elektrycznej płycie grzejnej (odradzam stosowanie kuchenki gazowej, otwartego ognia, jeśli jednak nie mamy
wyjścia, pierdolimy BHP) i grzejemy do takiej temperatury w której zawartość naczynia reakcyjnego sobie bulgocze. Refluks kontynuujemy przez około 45 minut do godziny.
Po tym czasie mamy prawie pewność że całość p2np przereagowała. Mieszanina w tym momencie może mieć kolor od szarego przez zgniło zielony do prawie czarnego.
Zauważymy, że większość foli została zjedzona.
Kolejnym etapem jest alkalizacja, czyli wyparciej wolnej zasady amfetaminy sprowadzając mieszaninę do zasadowego ph (10-12) używając roztworu wodorotlenku sodu.
Alkalizując musimy pamiętać, aby nie sprowadzić do ph>12, bo zniszczymy nasza wolną zasadę oraz robiąc roztwór wodorotlenku sodu nie dodać go zbyt dużo.
Jeśli dodamy do naszej mieszaniny zbyt nasycony roztwór, przyjmie ona postać gęstej zupy. Dodajemy wtedy wody. Przyrządzając r-r dobrze jest dodać do wody kostki
lodu i ostudzić go, ponieważ proces alkalizacji jest śilnie egzotermiczny i jeśli temperatura wzrośnie zbyt wysoko to spierdolimy to co co wcześniej zrobiliśmy.
Do dzieła!
Wodny roztwór wodorotlenku sodu (proporcje są takie, jednak to zbyt duża ilość jak na 5g p2np)
-woda 1l
-NaOH 300g
Alkalizacja:
Do naszej ciemnoszarej mieszaniny wlewamy porcjami roztwór NaOH silnie mieszając i uważając żeby całość się nie zagotowała (jeśli robimy to zbyt szybko,
zauważymy jak całość ciemnieje). Cały czas mierzymy ph. Jeśli jest pomiędzy 10-12 to ok. Jeśli nie, wiesz co robić. Gdy mieszanina osiągnie pożądane ph
zauważymy jak powstają nam dwie warstwy. Górna warstwa zazwyczaj ma kolor od pomarańczowego do czerwonego, jest to zależne od jakości odczynników i jest to
nasza amina w postaci wolnej zasady tzw. freebase. Zbieramy górną warstwę piperą/strzykawką i wylewamy np. do szklanki.
Odradzam rozdzielacz ponieważ zatka nam się kranik. Teraz musimy zebrać resztki aminy z dolnej warstwy, czyli tej co została w kolbie, ekstrachując
dwiema 20ml porcjami toluenu lub benzyny ekstrakcyjnej (ważne żeby rozuszczalnik był niepolarny). Czyli wlewamy naszą mieszaninę do plastikowej butelki,
dodajemy 20ml toluenu, zakręcamy butelke i całość trzepniemy przez kilka minut. Zbieramy Górną warstwę (toluenową, toluen jest mniej gęsty od wody)
i wlewamy do naczynia w kórym mamy wolną zasadę. Do butelki znów wlewamy 20ml toueny i robimy to samo co przed chwilą. To co mamy w butli jest do wyrzucenia.
Teraz dobrze byłoby oczyścić to co mamy.
Myjemy butelkę toluenem lub bierzemy drugą i wlewamy do niej nasze ekstrakty, czyli całość wolnej zasady w toluenie.
Dolewamy 50ml wody destylowanej i ekstrachujemy. Możemy w korku zrobić dziurkę, zatkać palcem i butelkę odwrócić. Zlewamy dolną warstwę (wodną),
a górną warstwę myjemy jeszcze raz 50ml wodą z solą i jeszcze raz 50ml samą wodą. Po wstępnym oczyszczeniu naszej zasady możemy ją jeszcze oddestylować
(wtedy wiemy że mamy czysty produkt) lub od razu przystępujemy do wysalania czyli wolną zasadę amfetaminy przekształcamy w naszym wypadku w siarczan amfetaminy.
A więc sprawa wygląda tak, że musimy zrobić roztwór kwasu siarkowego (możemy użyć elektrolitu) w IPA w stosunku 1:5-> 1ml kwasu i 5ml Ipa.
Roztwór kwasu wkraplamy strzykawką do r-r fety freebase w toluenie kropla po kropli intensywnie mieszając. Zauważymy, że pomarańczowy roztwór zacznie robić się
coraz bardziej biały, wytrącać się zacznie siarczan amfetaminy w formie krystalicznobiałego osadu. Gdy ph osiągnie wartość około 7 (obojętne),
odsączamy osad próżniowo na lejku buchnera, przemywając zimnym acetonem. Jeśli nie mamy lejka buchnera, odsączanie możemy przeprowadzić na filtrze do kawy.
Jeśli nie przemyjemy otrzymanego produkty może on mieć kolor różowy.
W ten sposób otrzymaliśmy około 3g siarczanu amfetaminy, który możemy wymieszać w stosunku 1:1 np. z kretem, czerwonym fosforem, strychniną, rtęcią lub ołowiem a i tak siła będzie zabójcza! Uważajcie na siebie i wylewajcie rtęć do kanalizacji!
polecam przyjżeć się temu
Tutorial zamieszczam w celach jedynie informacyjnych, produkcja amfetaminy jest nielegalna a całość to jedynie moje domysły!
po prostu nie wychodzi, postanowiłem wyjść z pomocą. Głównym powodem dla którego po zmieszaniu amalgamatu z esencją octową, ipa i p2np nie dzieje się nic
jest brak amalgamatu na powierzchni aluminium. Dzieje się tak, ponieważ folia aluminiowa jest zbyt cienka, i albo jest zjadana podczas amalgowania,
albo wymywamy amalgamat przepłukując go wodą. Można tego uniknąć na dwa sposoby.
1. użyć grubszego źródła aluminium (np. aluminiowe tacki do grilla)
2. redukować i amalgować jednocześnie.
Ja skupię się na metodzie drugiej. Cała reakcja wygląda tak, że do 1l kolby lub słoika wsypujemy:
-pociętą w trójkąty równoramienne folię aluminiową w ilości 8g
-P2NP;fenylonitropropen 5g
-IPA;izopropanol 50ml (do kupienia w sklepach komputerowych, jest używany do czyszczenia)
-esencja octowa (kwas octowy 80%) 50ml (ewentualnie rozcieńczyć lodowaty kwas octowy)
-HgCl2; chlorek rtęci (III) 30mg (ilość możecie dobrać doświadczalnie, lepiej nie dawać więcej jeśli robicie duże ilości ponieważ całość wypierdoli z kolby)
Jeśli jest możliwość zakładamy na kolbę chłodnicę w trybie zwrotnym, czyli pionowo, i odpalamy przepływ wody przez nią, jeśli nie mamy to nie zakładamy.
Po kilku minutach nasza mieszanina zaczyna się nagrzewać, wtedy powinniśmy całość wymieszać ponieważ p2np rozpuszcza sie w ciepłych rozpuszczalnikach.
Gdy p2np się rozpuści, naszą kolbę lub słoik wsadzamy do garnka/wiadra/wanny/kibla/przerębla/rzeki z zimną wodą. Jest to konieczne bo gdy reakcja się rozpędza,
całość zaczyna się mocno nagrzewać, tak że nawet nie będziemy w stanie utrzymać kolby w ręce, poza tym całość może wyjebać poza kolbę.
Zanurzając kolbę lub słoik w wodzie kontrolujemy reakcję, jeśli widzimy, że całość mieści się w naczyniu, wyciągamy je. Po około 10-15 minutach większość
fenylonitropropenu jest już zredukowana jednak my chcąc zwiększyć wydajność naszej reakcji, wsadzamy nasze naczynie reakcyjne (słoik lub kolba) do łaźni wodnej,
czyli do garnka z wodą lub olejem, który kładziemy na elektrycznej płycie grzejnej (odradzam stosowanie kuchenki gazowej, otwartego ognia, jeśli jednak nie mamy
wyjścia, pierdolimy BHP) i grzejemy do takiej temperatury w której zawartość naczynia reakcyjnego sobie bulgocze. Refluks kontynuujemy przez około 45 minut do godziny.
Po tym czasie mamy prawie pewność że całość p2np przereagowała. Mieszanina w tym momencie może mieć kolor od szarego przez zgniło zielony do prawie czarnego.
Zauważymy, że większość foli została zjedzona.
Kolejnym etapem jest alkalizacja, czyli wyparciej wolnej zasady amfetaminy sprowadzając mieszaninę do zasadowego ph (10-12) używając roztworu wodorotlenku sodu.
Alkalizując musimy pamiętać, aby nie sprowadzić do ph>12, bo zniszczymy nasza wolną zasadę oraz robiąc roztwór wodorotlenku sodu nie dodać go zbyt dużo.
Jeśli dodamy do naszej mieszaniny zbyt nasycony roztwór, przyjmie ona postać gęstej zupy. Dodajemy wtedy wody. Przyrządzając r-r dobrze jest dodać do wody kostki
lodu i ostudzić go, ponieważ proces alkalizacji jest śilnie egzotermiczny i jeśli temperatura wzrośnie zbyt wysoko to spierdolimy to co co wcześniej zrobiliśmy.
Do dzieła!
Wodny roztwór wodorotlenku sodu (proporcje są takie, jednak to zbyt duża ilość jak na 5g p2np)
-woda 1l
-NaOH 300g
Alkalizacja:
Do naszej ciemnoszarej mieszaniny wlewamy porcjami roztwór NaOH silnie mieszając i uważając żeby całość się nie zagotowała (jeśli robimy to zbyt szybko,
zauważymy jak całość ciemnieje). Cały czas mierzymy ph. Jeśli jest pomiędzy 10-12 to ok. Jeśli nie, wiesz co robić. Gdy mieszanina osiągnie pożądane ph
zauważymy jak powstają nam dwie warstwy. Górna warstwa zazwyczaj ma kolor od pomarańczowego do czerwonego, jest to zależne od jakości odczynników i jest to
nasza amina w postaci wolnej zasady tzw. freebase. Zbieramy górną warstwę piperą/strzykawką i wylewamy np. do szklanki.
Odradzam rozdzielacz ponieważ zatka nam się kranik. Teraz musimy zebrać resztki aminy z dolnej warstwy, czyli tej co została w kolbie, ekstrachując
dwiema 20ml porcjami toluenu lub benzyny ekstrakcyjnej (ważne żeby rozuszczalnik był niepolarny). Czyli wlewamy naszą mieszaninę do plastikowej butelki,
dodajemy 20ml toluenu, zakręcamy butelke i całość trzepniemy przez kilka minut. Zbieramy Górną warstwę (toluenową, toluen jest mniej gęsty od wody)
i wlewamy do naczynia w kórym mamy wolną zasadę. Do butelki znów wlewamy 20ml toueny i robimy to samo co przed chwilą. To co mamy w butli jest do wyrzucenia.
Teraz dobrze byłoby oczyścić to co mamy.
Myjemy butelkę toluenem lub bierzemy drugą i wlewamy do niej nasze ekstrakty, czyli całość wolnej zasady w toluenie.
Dolewamy 50ml wody destylowanej i ekstrachujemy. Możemy w korku zrobić dziurkę, zatkać palcem i butelkę odwrócić. Zlewamy dolną warstwę (wodną),
a górną warstwę myjemy jeszcze raz 50ml wodą z solą i jeszcze raz 50ml samą wodą. Po wstępnym oczyszczeniu naszej zasady możemy ją jeszcze oddestylować
(wtedy wiemy że mamy czysty produkt) lub od razu przystępujemy do wysalania czyli wolną zasadę amfetaminy przekształcamy w naszym wypadku w siarczan amfetaminy.
A więc sprawa wygląda tak, że musimy zrobić roztwór kwasu siarkowego (możemy użyć elektrolitu) w IPA w stosunku 1:5-> 1ml kwasu i 5ml Ipa.
Roztwór kwasu wkraplamy strzykawką do r-r fety freebase w toluenie kropla po kropli intensywnie mieszając. Zauważymy, że pomarańczowy roztwór zacznie robić się
coraz bardziej biały, wytrącać się zacznie siarczan amfetaminy w formie krystalicznobiałego osadu. Gdy ph osiągnie wartość około 7 (obojętne),
odsączamy osad próżniowo na lejku buchnera, przemywając zimnym acetonem. Jeśli nie mamy lejka buchnera, odsączanie możemy przeprowadzić na filtrze do kawy.
Jeśli nie przemyjemy otrzymanego produkty może on mieć kolor różowy.
W ten sposób otrzymaliśmy około 3g siarczanu amfetaminy, który możemy wymieszać w stosunku 1:1 np. z kretem, czerwonym fosforem, strychniną, rtęcią lub ołowiem a i tak siła będzie zabójcza! Uważajcie na siebie i wylewajcie rtęć do kanalizacji!
polecam przyjżeć się temu
Tutorial zamieszczam w celach jedynie informacyjnych, produkcja amfetaminy jest nielegalna a całość to jedynie moje domysły!
TO ŻE ZADZIAŁAŁO I DZIAŁA TAK NA MNIE WCALE NIE ZNACZY ZE PODZIAŁA TAK NA CIEBIE.
ਚਾਰ EM EM ਈਸਵੀ
څلور em em ce
አራት ኤም ኤም ዓ.ም.
ਚਾਰ EM EM ਈਸਵੀ
څلور em em ce
አራት ኤም ኤም ዓ.ም.
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
O kurde, panie to teraz czekam na "domysła" dotyczącego twojego snu jak zrobić 4mmc
Testy i badania substancji opisywanych przez mnie, są prowadzone za granicą, w takich krajach jak Słowacja i Holandia.
W Polsce większość substancji opisywana przez mnie, jest nielegalna, dlatego tutaj badań nie prowadzę.
W Polsce większość substancji opisywana przez mnie, jest nielegalna, dlatego tutaj badań nie prowadzę.
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
a skąd wziąć chlorek rtęci ? na alledrogo jest niby 100 g za 110 złociszy , ale jak ja potrzebuje tylko 30 mg to po co mi aż tyle tego ;p może być jakiś zamiennik ?
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
chciałem zapytać o coś. Mianowicie nie ważne którą metodę wybiorę , Twoją czy swima to i tak zawsze coś spierdole i problem ze nie wiem kiedy i gdzie. A trudne niby nie jest. Po reakcji kwasu octowego (mam 80% wiec dodaje go 70 ml i 5ml wody destylowanej), P2np, ipa i Alu - nie wazne czy samego amalgamatu czy tez razem z hgcl2 za każdym razem mam ciemnoszara miksturę , daje refluks i.... to się nigdy nie robi jaśniejsze, po godzinie dalej ciemnoszary mix, identyczny jak przed refluxem. Spójny, jednowarstwowy. 5 prób i ... to samo. Ale nawet się tym już zbytnio nie przejmując , próbuje iść dalej i dodając naoh 50g z 50ml wody, znowu jest problem w którymś momencie przy dodawaniu zauważam(czasem ) ze ta folia się jakby znowu zżera ( bo nigdy nie zjada się do końca wcześniej) i wtedy zazwyczaj podczas mieszania nagle się wszystko robi czarne jak Cola . I co wtedy? Napisałeś, ze jak pH jest 10 do12 to jeśli nie - wiesz co robić, no taaa.... ale czekaj... ja niestety nie wiem, co więcej chciałem zapytać jeszcze o te kostki lodu ze niby kiedy i jak i użyć ? Ja nie mogę ruszyć dalej z eksperymentem. Proszę o pomoc
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
Nie myć aluminium, bez chlorku rtęci, metal nie topi się. Nauczyłem się tego od 4mmc. Dziękuję Ci. Do tej pory mam mokrą różową pastę. Suszenie na moim balastu 400W, obok namiotu chwastów lol.
Dont wash aluminium, without mercury chloride, metal will not melt. I learned this from 4mmc. Thank you. So far I have wet pink paste. Drying on my 400w ballast, next to my weed tent lol.
Dont wash aluminium, without mercury chloride, metal will not melt. I learned this from 4mmc. Thank you. So far I have wet pink paste. Drying on my 400w ballast, next to my weed tent lol.
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
nowa synteza p2np do amfetaminy przetłumaczone z rosyjskiego Mam nadzieję, że ludzie uznają to za pomocne to nie moja praca nie mogę ubiegać się o kredyt
AMPHETAMINE SYNTHESIS IS CORRECTLY
Russian Method (Translated)
There are many descriptions of this synthesis, but unfortunately they do not describe in detail
the chemistry of the process, and not understanding what you are doing and why it is difficult to achieve high and consistent results of the synthesis. I will try to correct this situation. And at the same time I will give practical
recommendations on key points, often I repeat with them, but repetition is the mother of learning. And it is more convenient when everything is in one place. Some places may be boring, sometimes clumsy, but I think generally informative. Do not judge strictly, he wrote as he could.
At the beginning in general terms.
In our case, the reduction of 1-phenyl-2-nitropropene (p2np) occurs atomic hydrogen (whose activity is much higher than the molecular activity) released by the reaction of aluminum with water and acetic acid in the presence of mercury as a catalyst. Since the lifetime of atomic hydrogen is not large, and the bulk of mercury is on aluminum in the form of amalgam, directly in the reaction zone and the bulk of the reduction occurs there. Therefore, it is not good when the amalgam in the flask floats from above above the solvent with p2np, a part of the hydrogen flies away to the idle. It is necessary to shake up the contents of the flask in order to achieve a uniform distribution of the amalgam in the reaction mass (PM) to involve all p2np in the reduction process. But this is of course when the reaction subsides, at the beginning is usually not up to it.
More on what is happening there.
In the reaction of aluminum and mercury (amalgamation), the latter is introduced in the form of a solution of a bivalent salt, in our country it is most often nitrate. At the same time, aluminum from oxide reduces mercury from nitrate:
2 AlO3 + 3 Hg (NO3) 2 = 3 Hg + 2 Al (NO3) 3 + 3 O2
The resulting metallic mercury adheres to the following layer of aluminum to form amalgam:
Al + Hg = (Al, Hg),
Aluminum directly from the amalgam reacts with water to form hydroxide:
2 (Al, Hg) + 6 H2O = 2 Al (OH) 3 + 3 H2 + 2 Hg (black dregs)
and in the case of a reduction reaction with acetic acid to form aluminum acetate:
2 (Al, Hg) + 6 CH3COOH = 2 Al (C2H3O2) 3 +3 H2 + 2 Hg and most likely its subsequent hydrolysis to basic aluminum acetate Al (OH) (CH3COO) 2
in all these reactions, the hydrogen required for reduction is released, and mercury adheres to the next layer of aluminum, and so on until it completely reacts. As a result, aluminum compounds forming at the end will form a dense gray mass with residual water, vinegar, solvent and hydrogen bubbles, which still contains metallic mercury left over from the decomposition of amalgam. The results of possible adverse reactions are not taken into account.
Requirements for amalgam and its manufacturing process.
The intensity of the reaction depends on the area of the reacting foil, the degree and quality of the formation of its surface amalgam. Duration depends on the latter in the place with foil thickness.
First about the foil. Accordingly, the thinner the foil, the more it should be cut to the required weight, and the greater the area of the reaction. Hence the opportunity not to keep it at the beginning, or not to get it properly because of the reaction of the majority of aluminum in the amalgamation process. The most common foil thickness is 9 microns, it is Chinese gavno 6 microns, there is "Sayan" 11 microns, "Sayan extra-strong" 14 microns and for a grill 20 microns. For a moderately active and long-lasting reaction and to prevent the possibility of perederzhat amalgam before the premature completion of the reaction, it makes sense to take a thicker. And how much to take (this is individual): for p2np, they usually take in the amount of from 1: 1 to the weight of the propene pledged to 1: 1.5. For more heavily reduced substituted propenes, nitrostyrenes and nitrosterenes with an excess of 1.5-2 times. The thicker the foil, the more abundant it is taken, and the exact number is already selected for itself with experience.
Now about the reaction itself. It is better to control the process by the state of the foil itself, it should lose its luster (become matte) and become covered with gray spots. The completely gray foil reacts very violently, this is appropriate only with the above-mentioned difficult-to-repair compounds, with not large tabs. In general, the color rendition is an individual thing, which for one already seems dull - for another it is still brilliant. For starters, it is better to first drive the amalgam all the way to idle, look at the process, detect the desired state, and make a synthesis from it, and if it is successful, increase the bookmarks.
For even contact of Al and Hg, the foil is recommended to be degreased - it was completely covered in the process of cutting with microlayer of fat from the fingers. To do this, usually use washing tech. Acetone.
But the trick is that Hg (NO3) 2 dissolves in acetone better than in water (in it and in IPSe its solubility is considered limited). Directly pour the foil with a solution of Hg (NO3) 2 in the acic, we splutter up by doing so 2 operations at once - degreasing and directly pouring mercury solution onto the foil. And we also catch additional advantages: in the foil, the foil decomposes slowly, there is little sludge - it is easier to monitor its condition, and it is difficult to gape and overexpose to a penetrating (but not violent) reaction. The speed of the process depends on the concentration of mercury in the solution and to a lesser extent on the temperature of the solvent, if it is usually t room + several degrees. For accurate dosage of Hg (NO3) 2, it should be in a more or less pure form. How to make soluble mercury salts correctly. See here - Please login or register to view the hidden text.
At the end of the reduction reaction, we have the above-described sludge, from which it is necessary to get the amine, which is in the form of acetate, our further actions are called acid-base extraction or simply kaschey. It is based on the different solubilities of the bases and salts of organic compounds in different solvents. Salts are readily soluble in water, some are sparingly soluble in polar solvents and insoluble in non-polar ones. The bases are insoluble in water and soluble in organic solvents. Being in a vessel with two not miscible solvents, the substance tends to the one where its solubility is higher.
And so, alkalization is carried out, and that this comes from the interesting and important of the reactions with NaOH:
NaOH removes acid residue from amine acetate and converts it to the free base; it is the only reaction product soluble in organic solvents
mercury nitrate goes into non-toxic oxide - Hg (NO3) 2 + 2 NaOH = HgO + 2 NaNO3 + H2O
with acetic acid CH3COOH + NaOH = CH3COONa + H2O
Remaining aluminum and aluminum hydroxide reacts with NaOH with sodium aluminates at the outlet:
2Al + 2NaOH + 6H2O = 2Na [Al (OH) 4] + 3H2 and Al (OH) 3 + 3NaOH = Na3 [Al (OH) 6]
Concentrated alkali solution pushes IPA with amine out of itself, but it is not recommended to immediately select it and sour it. The separation of the layers after alkalization is not a complete IPA obtained by us contains a decent amount of water, and in the remaining layer of water / sludge also remains ips in a decent concentration, which holds the base of the amine. Plus, the remaining mercury nitrate probably dissolves to a limited extent in ipsa. Also, NaOH dissolves directly in IPSe, approximately 10 g / 100 ml. Water in the ice not only carries dirt into the finished product, but also significantly reduces the yield by dissolving the finished product, and alkali it boils with the corresponding sodium salt.
Here is a method for getting an amine without water. The base of amine is obtained by a non-polar, water-immiscible solvent. So cut off the water and dirt. Perfect n-Pentane, petroleum ether 40-70 is good. In ordinary chemmags, they are not as expensive as ips and pure acetone. If you don't get to himmaga we beat out toluene from 646th. Some practitioners believe that it is even preferable. Just pour water into it and toluene floats up, it's 50% there, a mixture of water, acetone and methanol below. Method: conducted a reaction with 100ml of source code, there is a separation of layers; diluted with a liter of water, the separation disappears and ips in the resulting concentration of amine is actually not able to hold. Pour 100 ml of water there not polar and shake vigorously for at least 3 minutes, separate it. Repeat well with 50ml. We obtain 150 ml of a non-polar solvent, which absorbed only all the amine from the Republic of Moldova. With large bookmarks, the amount of water to increase in proportion to the increase in bookmarks.
Dry the solution of amine in a nonpolar with anhydrous magnesium sulphate, dilute it in half with a polar solvent (ips or acetone from a chemical magma, worse than usual from a hardware store) and sour. For additional purification, you can rinse the obtained salt, or repeat with your soup.
AMPHETAMINE SYNTHESIS IS CORRECTLY
Russian Method (Translated)
There are many descriptions of this synthesis, but unfortunately they do not describe in detail
the chemistry of the process, and not understanding what you are doing and why it is difficult to achieve high and consistent results of the synthesis. I will try to correct this situation. And at the same time I will give practical
recommendations on key points, often I repeat with them, but repetition is the mother of learning. And it is more convenient when everything is in one place. Some places may be boring, sometimes clumsy, but I think generally informative. Do not judge strictly, he wrote as he could.
At the beginning in general terms.
In our case, the reduction of 1-phenyl-2-nitropropene (p2np) occurs atomic hydrogen (whose activity is much higher than the molecular activity) released by the reaction of aluminum with water and acetic acid in the presence of mercury as a catalyst. Since the lifetime of atomic hydrogen is not large, and the bulk of mercury is on aluminum in the form of amalgam, directly in the reaction zone and the bulk of the reduction occurs there. Therefore, it is not good when the amalgam in the flask floats from above above the solvent with p2np, a part of the hydrogen flies away to the idle. It is necessary to shake up the contents of the flask in order to achieve a uniform distribution of the amalgam in the reaction mass (PM) to involve all p2np in the reduction process. But this is of course when the reaction subsides, at the beginning is usually not up to it.
More on what is happening there.
In the reaction of aluminum and mercury (amalgamation), the latter is introduced in the form of a solution of a bivalent salt, in our country it is most often nitrate. At the same time, aluminum from oxide reduces mercury from nitrate:
2 AlO3 + 3 Hg (NO3) 2 = 3 Hg + 2 Al (NO3) 3 + 3 O2
The resulting metallic mercury adheres to the following layer of aluminum to form amalgam:
Al + Hg = (Al, Hg),
Aluminum directly from the amalgam reacts with water to form hydroxide:
2 (Al, Hg) + 6 H2O = 2 Al (OH) 3 + 3 H2 + 2 Hg (black dregs)
and in the case of a reduction reaction with acetic acid to form aluminum acetate:
2 (Al, Hg) + 6 CH3COOH = 2 Al (C2H3O2) 3 +3 H2 + 2 Hg and most likely its subsequent hydrolysis to basic aluminum acetate Al (OH) (CH3COO) 2
in all these reactions, the hydrogen required for reduction is released, and mercury adheres to the next layer of aluminum, and so on until it completely reacts. As a result, aluminum compounds forming at the end will form a dense gray mass with residual water, vinegar, solvent and hydrogen bubbles, which still contains metallic mercury left over from the decomposition of amalgam. The results of possible adverse reactions are not taken into account.
Requirements for amalgam and its manufacturing process.
The intensity of the reaction depends on the area of the reacting foil, the degree and quality of the formation of its surface amalgam. Duration depends on the latter in the place with foil thickness.
First about the foil. Accordingly, the thinner the foil, the more it should be cut to the required weight, and the greater the area of the reaction. Hence the opportunity not to keep it at the beginning, or not to get it properly because of the reaction of the majority of aluminum in the amalgamation process. The most common foil thickness is 9 microns, it is Chinese gavno 6 microns, there is "Sayan" 11 microns, "Sayan extra-strong" 14 microns and for a grill 20 microns. For a moderately active and long-lasting reaction and to prevent the possibility of perederzhat amalgam before the premature completion of the reaction, it makes sense to take a thicker. And how much to take (this is individual): for p2np, they usually take in the amount of from 1: 1 to the weight of the propene pledged to 1: 1.5. For more heavily reduced substituted propenes, nitrostyrenes and nitrosterenes with an excess of 1.5-2 times. The thicker the foil, the more abundant it is taken, and the exact number is already selected for itself with experience.
Now about the reaction itself. It is better to control the process by the state of the foil itself, it should lose its luster (become matte) and become covered with gray spots. The completely gray foil reacts very violently, this is appropriate only with the above-mentioned difficult-to-repair compounds, with not large tabs. In general, the color rendition is an individual thing, which for one already seems dull - for another it is still brilliant. For starters, it is better to first drive the amalgam all the way to idle, look at the process, detect the desired state, and make a synthesis from it, and if it is successful, increase the bookmarks.
For even contact of Al and Hg, the foil is recommended to be degreased - it was completely covered in the process of cutting with microlayer of fat from the fingers. To do this, usually use washing tech. Acetone.
But the trick is that Hg (NO3) 2 dissolves in acetone better than in water (in it and in IPSe its solubility is considered limited). Directly pour the foil with a solution of Hg (NO3) 2 in the acic, we splutter up by doing so 2 operations at once - degreasing and directly pouring mercury solution onto the foil. And we also catch additional advantages: in the foil, the foil decomposes slowly, there is little sludge - it is easier to monitor its condition, and it is difficult to gape and overexpose to a penetrating (but not violent) reaction. The speed of the process depends on the concentration of mercury in the solution and to a lesser extent on the temperature of the solvent, if it is usually t room + several degrees. For accurate dosage of Hg (NO3) 2, it should be in a more or less pure form. How to make soluble mercury salts correctly. See here - Please login or register to view the hidden text.
At the end of the reduction reaction, we have the above-described sludge, from which it is necessary to get the amine, which is in the form of acetate, our further actions are called acid-base extraction or simply kaschey. It is based on the different solubilities of the bases and salts of organic compounds in different solvents. Salts are readily soluble in water, some are sparingly soluble in polar solvents and insoluble in non-polar ones. The bases are insoluble in water and soluble in organic solvents. Being in a vessel with two not miscible solvents, the substance tends to the one where its solubility is higher.
And so, alkalization is carried out, and that this comes from the interesting and important of the reactions with NaOH:
NaOH removes acid residue from amine acetate and converts it to the free base; it is the only reaction product soluble in organic solvents
mercury nitrate goes into non-toxic oxide - Hg (NO3) 2 + 2 NaOH = HgO + 2 NaNO3 + H2O
with acetic acid CH3COOH + NaOH = CH3COONa + H2O
Remaining aluminum and aluminum hydroxide reacts with NaOH with sodium aluminates at the outlet:
2Al + 2NaOH + 6H2O = 2Na [Al (OH) 4] + 3H2 and Al (OH) 3 + 3NaOH = Na3 [Al (OH) 6]
Concentrated alkali solution pushes IPA with amine out of itself, but it is not recommended to immediately select it and sour it. The separation of the layers after alkalization is not a complete IPA obtained by us contains a decent amount of water, and in the remaining layer of water / sludge also remains ips in a decent concentration, which holds the base of the amine. Plus, the remaining mercury nitrate probably dissolves to a limited extent in ipsa. Also, NaOH dissolves directly in IPSe, approximately 10 g / 100 ml. Water in the ice not only carries dirt into the finished product, but also significantly reduces the yield by dissolving the finished product, and alkali it boils with the corresponding sodium salt.
Here is a method for getting an amine without water. The base of amine is obtained by a non-polar, water-immiscible solvent. So cut off the water and dirt. Perfect n-Pentane, petroleum ether 40-70 is good. In ordinary chemmags, they are not as expensive as ips and pure acetone. If you don't get to himmaga we beat out toluene from 646th. Some practitioners believe that it is even preferable. Just pour water into it and toluene floats up, it's 50% there, a mixture of water, acetone and methanol below. Method: conducted a reaction with 100ml of source code, there is a separation of layers; diluted with a liter of water, the separation disappears and ips in the resulting concentration of amine is actually not able to hold. Pour 100 ml of water there not polar and shake vigorously for at least 3 minutes, separate it. Repeat well with 50ml. We obtain 150 ml of a non-polar solvent, which absorbed only all the amine from the Republic of Moldova. With large bookmarks, the amount of water to increase in proportion to the increase in bookmarks.
Dry the solution of amine in a nonpolar with anhydrous magnesium sulphate, dilute it in half with a polar solvent (ips or acetone from a chemical magma, worse than usual from a hardware store) and sour. For additional purification, you can rinse the obtained salt, or repeat with your soup.
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
Synteza jest dobrze opisana na pewnym forum dotyczącym chemi "teoretycznej" poszukaj to znajdziesz, trochę bezczelnym było by wklejenie tego opisu (a właściwie dwóch) no ale z drugiej strony może by się nie obrazili, w końcu gdyby tamto forum padło, dobrze mieć kopie zapasową
W badaniach nie biorą udziału zwierzęta!
Not tested on animals!
Not tested on animals!
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
Kokaspaniel, po wpisaniu odpowiedniej frazy w google jest nawet wersja z fotkami i obrazkami.
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
Amphetamine Sulphate Bible.
Not my work, trancelated from russian.
(Use google trancelate for desired Language)
"P2NP Russian Methods."
Main Points
1. Do not rinse aliminium, this makes it impossible to melt the aluminium.
2. Reaction Mixtue Should be grey, not white or Pink, deliberate lies by law enforcement.
3. Sodium Hydroxide is essential. Sodium Bicarbonate will not give you anything more than weak cocaine effect, a drug for assholes.
"The most widely used reaction is the synthesis of amphetamine from phenylacetone. It is distinguished by the fact that the synthesis is easily scaled to large volumes of loading, at least 100 kg, and to obtain a pure product at the output. But unfortunately in the Russian Federation the main source component - phenylacetone, is on the lists of narcotic substances, so its purchase is impossible due to its illegal status. All companies that are engaged in the production and marketing of phenylacetone have stopped this activity with the release of the ban."
Nowadays, the most common method of synthesis is the condensation of benzaldehyde with nitroethane in the presence of a catalyst to form 1-phenyl-2-nitropropene, which is then reduced by mercury-aluminum amalgam.
In 2014, nitroethane, benzaldehyde and 1-phenyl-2-nitropropene were added to table 1 of the list of precursors, which significantly complicated the purchase of source codes.
Before the ban, the main source could be bought at a price of 5k per kg of nitroethane and 2k per kg of benzaldehyde. From the bookmark of 1 kg of BA and 1 kg of NE, it turned out to be slightly more than 1 kg of 1-phenyl-2-nitropropene, which, taking into account the catalyst (cyclohexylamine, butylamine or ammonium acetate) and isopropyl alcohol, was released at a cost of 8-9 thousand rubles for cleaning. In this scenario, the final cost of the finished product was 18 000 rubles.
Currently, it is rather difficult to buy source codes for phenylnitropropene, therefore we offer the option of purchasing ready-made PNP in solution, or its legal counterparts, such as phenylnitropropane.
The price for 1kg on the Internet varies from 35k to 50k, respectively, when buying in bulk additional discounts.
In addition to the main source, we will need other reagents. To load 1kg of FNP with an average cost of 40k you need:
5 kg of acetic acid 170r per kg
10l of isopropyl alcohol 150r per liter when buying from 10l
A few grams of mercury salt, which is obtained from metallic mercury from thermometers and nitric acid (200r per liter), thermometers 1.5k
1.2 kg of chopped aluminum foil (60r per roll, 17 rolls)
3 kg of sodium alkali at 130p per kg
100ml of sulfuric acid at 100r per kg
2l acetone 200r per kg
Given the average yield of 70% (without additional manipulations to increase output), the average cost of amphetamine with this method of synthesis is 65,000 rubles (slightly more than $ 1,000)
The price review was conducted in October 2015.
In addition to chemical reagents, we need the simplest equipment, laboratory glass and consumables:
Vacuum pump with 5l Bunsen flask and Buchner funnel - for filtering and washing the finished salt. (8000r per set)
"This kit will help to collect in any chemical store."
Laboratory or kitchen scales (preferably with a calibration weight)
Flat-bottomed 6l flasks with 45 - 4-5 pieces (3000r per pc)
Reverse ball refrigerators loop 45 - 4-5 pieces (2000r per piece)
Basins for cooling flasks during recovery (reaction with a large amount of heat that needs to be kept) (500r per pc)
Different volume laboratory glasses, in the sizes and forms convenient for the cooker. (all glasses can be bought for 3000r)
Alkali Bucket (1000r)
Plastic barrel into which the amalgam held by the conveyor belt will merge (3000)
Latex gloves (200r per pack)
Gauze, or a sieve for draining mercury solution (100r)
Litmus test strips (200r per pack)
Shredder paper shredder (4000r)
Trays for drying the finished product (200r apiece)
20 vat syringes without elastic at the end of the piston (20p per pc)
Desalting Buchner funnel filters (white ribbon) (250r per pack)
To protect clothes a bathrobe (500 rubles) or a painting suit.
Mask with goggles for eye protection and breathing (3000) (3M Mask for Mercury Vavours, Filters should be square pink)
In total, we need about 50,000 rubles to equip the laboratory with glass and equipment.
Additional spending on consumables 1000r
Chemical reagents, equipment and consumables can be purchased at retailers chemical reagents.
All stores are controlled by the authorities, so everything in one place is not worth buying.
Anonymously, but at more expensive prices, you can buy on the forums from Chembro and Mechanics.
A small digression. In this article, we look at the synthesis method in a schematic way. For those who do not have experience assembling amphetamine, you must first get your hand on small quantities, and only then to plan the scaling of the synthesis.
For the first “call to brew”, we recommend that you contact ChemBro or Mechanic’s stores to purchase the assembled “Lego” kit and get technical advice on assembly.
Preparation of the room.
For the work we need a suitable place. The summer cottage is ideal, but you can consider options for placing in the industrial zone, or in the garage. Due to the large odor emission, the apartment is definitely not suitable. There will be enough 20 square square for us, but you can also have a larger area. The presence of electricity is not necessary, but desirable. It is important that the room is well ventilated (windows, or the presence of hoods).During the work we need a fairly large amount of water.
If there is no plumbing and sewage in the room, you will have to bring water and take away waste (for example, if you work in a garage). As a separate article, we will look at cooking in different types of premises in detail, tell you how to equip the space, arrange the equipment, do the drying, whom to arrange, how to preserve anonymity, disguise work and smells.
After you have mastered the laboratory synthesis in small quantities, prepared the premises for the work, purchased the necessary raw materials, equipment, glass, consumables, improvised means and chemical protection, you can start working on amphetamine in large quantities. By a large number, we mean the production of 1kg per day. You can work alone, but for safety, convenience, and increasing the speed of the process it is better to work together.
The whole synthesis process can be divided into several stages:
training
recovery
alkaline
⁃sour
drying and packaging.
During preparation, you need to bring all the reagents and equipment, look around for the presence of pale, cut the foil in advance with a paper shredder (you can immediately hang them in bags), prepare mercury nitrate.
Recovery.
To get 1kg of ready-made amphetamine, we need to supply 1400g of phenylnitpropene. Download all the weight in one tab can not be due to a complex reaction that does not scale well. Therefore, this process is broken down into many, many small tabs, for example, 50g in 6 l flasks. In general, we will need to put 28 flasks (1400g of propene), each of which will take about 40 minutes. Who has enough experience, can increase the working volume of flasks to 10 liters with a load of 70-100gr source. If you work together, you can immediately put 2-3 flasks, which will significantly speed up the process.
The process itself: we take a 6 l flask, pour 60 g of chopped foil into it, pour water over it so that it covers the entire foil and add a pinch of mercury salt. If you have mastered the synthesis in small quantities, you should be well aware of the signs of the finished amalgam. While it is infused, it is necessary to prepare a solution of 50g of PNP + 500ml IPA + 250ml of glacial acetic acid in a laboratory glass.The solution can be slightly heated to dissolve FNP. When the amalgam is ready, we pour out an aqueous solution of mercury salt (for convenience we use a sieve), then add half of the prepared solution of FNP + IPA + LUK to the flask with a fake and close with a reflux condenser (before each new reaction, cold water should be poured into the jacket of the refrigerator, and the nipples should be closed) hose clamps, clamped at the ends, or in the presence of running water, connect a full circulation. These measures will help to avoid excessive evaporation of the IPSa during a violent reaction).Immediately after the bay, a violent exothermic reaction begins (with a large amount of heat). To prevent overheating, the reaction mass should be cooled in a previously prepared basin of water. As soon as the reaction starts to decline, pour the half of the FNP solution remaining in the glass and wait for the reaction to complete. Those who have enough experience and believe in themselves, can immediately pour the entire solution of PNP. In this case there will be a more violent reaction that needs to be carefully controlled. Upon completion of the reaction, which is determined by the attenuation of the process and the dissolution of the foil, the entire reaction mass is poured into a 100 liter drum.
This is the hardest part of the process. Conveyor method need to rotate 28 syntheses of 50g. You can take a smaller amount, it all depends on the needs, for example, to reduce the planned output by half, that is, by 500g of the finished amphetamine. Then we will need to put 700gr source.
Alkalization
Alkalization is the simplest process in all synthesis. Alkaline we will be in a 100l barrel previously prepared cold alkali solution. The solution is prepared as follows: take a bucket, pour 4.5 kg of alkali into it, fill it with water until the alkali dissolves, usually 7l is enough. Immediately begins abundant heat. We wait until it cools, stirring occasionally. Cooling may take up to 2 hours.
Before alkalization, unreacted aluminum should be collected in the barrel with the reaction mass. This can be done by filtering the entire reaction mass through gauze or a sieve. If this is not done, the foil will react with alkali, additionally heating the mixture and releasing by-products.
Then in small portions gradually pour cold alkali into the RM. Warming up and subsequent separation into layers will begin. We need to carefully collect the entire top layer - this is ready-made amphetamine as a base, a solution in alcohol.
The bottom layer is sludge, in which 10% -20% of the product remains, which can be obtained by extraction. Extract with solvent, evaporate and combine with base oil. Pour the sludge, it is no longer needed.
Souring.
Probably the most interesting and important process. It is most convenient to sour in a wide laboratory glass of 500-1000ml. In a 250ml glass we prepare a solution of sulfuric acid in acetone (for 1ml of sulfur, 15ml of acetone). We pour a quarter of a glass with the base of phenamine and gradually, in small portions, from a 20 ml syringe, add our solution of sulfuric acid in acetone. Amphetamine sulphate flakes will start to fall.Sour gently to pH 5.5. If the mixture thickens strongly, then dilute it with a small amount of acetone so that there is no local over-acidification. If you peroxide, you can lose the whole product. So we have to acidify all the oil. Next, you need to thoroughly rinse the mass with acetone and press on the vacuum filtration system.
Drying & Packaging.
The washed and pressed product is unloaded on trays, dried at room temperature until completely dry. We weigh the dry, crumbly product and pack it in the necessary packing. We carry out cleaning of the room, we take out garbage.
We have dismantled the most popular at the moment the synthesis of amphetamine. At first glance, the process looks confused, with its difficulties. But with the proper approach and experience, everything goes coasting without any serious problems. A very big disadvantage of this method is the impossibility of scaling the reduction reaction. But even with the work in 6l-10l flasks, you can achieve monthly output of 15-30 kg in two cooks.
There are other ways to obtain this wonderful product, which we will keep in reserve in case of banning or withdrawing phenylnitropropene in solution and its analogues. Therefore, fans will accelerate the classics do not worry, for a long time you can pamper yourself with amphetamine.
SCALE PRODUCTION OF AMPHETAMINE
1 option proportions:
1 kg Phenylnitropropene (FNP) ~ 30000 - 50000r
3.5 kg Icy Acetic Acid (or 5kg 70% Acetic Essence) ~ 700-1000р
1.5kg Aluminum Foil (I recommend 11 microns thickness) ~ 1250r
30l Isopropyl Alcohol - less than 5000r
25 liters liters Petroleum ~ 4500r
Approximately 100ml Sulfuric Acid - less than 200r
8kg NaOH (Sodium Hydroxide, Alkali) - less than 1000r
Dry Mercury Nitrate or Mercury Nitrate Solution, obtained from 50 degree pharmacy and 100 ml of nitric acid (68%, density 1.4), followed by neutralization of excess acid drinking soda ~ 3000r
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TOTAL 45000-65000r = yield approximately 700g of pure amphetamine sulfate (cost 64000-93000 / 1kg)
2 variant proportions (I personally recommend it):
1kg Phenylnitropropene (FNP) - 30000-50000r
3.5 kg Icy Acetic Acid (or 5kg 70% Acetic Essence) ~ 700-1000р
1.5kg Aluminum Foil (I recommend 11 microns thickness) ~ 1250r
50l Ethyl acetate ~ 5000r
Approximately 100ml Sulfuric Acid - less than 200r
8kg NaOH (Sodium Hydroxide, Alkali) - less than 1000r
Dry Mercury Nitrate or Mercury Nitrate Solution, obtained from 50 degree pharmacy and 100 ml of nitric acid (68%, density 1.4), followed by neutralization of excess acid drinking soda ~ 3000r
TOTAL: 31000 - 61450 = Approximately 700g yield of amphetamine sulfate (cost 44300 - 87800r / kg)
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Mercury nitrate, cooking. (Skip if you have Mercury (ii) chloride)
Let's look at the wholesale manufacture of mercury nitrate for mass production of amphetamine.
In fact, to get mercury from thermometers is not dangerous and not scary, it is done elementary. First we put on gloves Option 1. A 2-liter dry glass is taken, narrow, placed on a hard surface (so as not to crack the glass), after which the thermometers are thrown tip-down. They naturally break, mercury flows out, you can knock a broken thermometer on the walls of the glass so that everything flows out, after which the thermometer is thrown into a prepared bucket next to it. The procedure is repeated 50 times (50 thermometers are broken into a glass).Next on the balcony \ in the open \ under the hood is installed stove. On the tile we put a glass with the extracted mercury, the tile is not included yet. Fill in a glass with 100 ml of nitric acid (density 1.4). The reaction begins with the release of brown vapor. Periodically stir everything with a glass rod, chasing balls of mercury. As soon as the reaction diminishes, we turn on the electric stove for a small power (Pts cannot be heated very much). The reaction to resume, mercury will gradually dissolve. If the temperature of PM is more than 50 degrees and the reaction does not go, we can add more nitric acid from the syringe, but in practice you never have to add more than 50 ml to 50 thermometers (i.e. + 1 ml per thermometer), most likely in such cases 5-10 ml will be enough. But, most likely, it will not be necessary to add it at all. The reaction is carried out until complete dissolution of mercury. After that, dilute the mixture with about 300 ml of water. Next, you need to neutralize the acid residues. To do this, in a glass, a LITTLE BIT (you can take a quarter of a teaspoon), add baking soda with vigorous stirring. Mixture
will foam strongly (carbon dioxide is released), soda will dissolve. Adding soda in small portions, continue until, after adding the next portion, an insoluble yellow color precipitate forms in the mixture. As soon as this happens, we collect nitric acid in the syringe and add it with DROPS with vigorous stirring until the precipitate dissolves. Now the mercury nitrate solution is neutralized. You may ask why this is necessary and why.
nitric acid cannot be infused with the calculation of "10 cubic meters per thermometer", as others advise - because excess acid in mercury nitrate solution (if you are not going to pour this nitrate solution into a crystallizer and get mercury nitrate in a dry form) can play a VERY cruel joke with you when preparing amalgam. Believe me, when it burns - it is very unpleasant, and if a piece of such foil comes into your hands - no gloves will help with severe burns).So, we have neutralized the mercury nitrate solution, now we dilute it with water in a glass to the 1 liter mark. IT IS VERY CONVENIENT. Since a liter of this solution will be consumed when recovering 1 kg of propene. Those. if we take a load of 50 g of PNP, then 75 g of foil will be processed to be used for its recovery, it will take 50 ml of this solution of mercury nitrate. Agree, it is convenient.
Option 2. Everything is the same as in option 1, just take a two-liter flask, lower the thermometer with the tip into the neck and have a snack with pliers, do it all with all the 50th thermometers, just pour nitric acid 100ml, heat it, dissolve the mercury, dilute it with water , neutralize with soda, bring the volume of the solution to 1 liter.
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Phenylnitropropene reduction 50 gram Batch! (amphetamine synthesis).
Method with isopropyl alcohol (IPA) and petroleum ether
Synthesis of 50 gram loading. Of course, cooks need to practice their skills at a load of 5-10 g of FNP in a 2 liter flask (you can easily count the proportions, the main truth is to start small. The synthesis is simple, but it requires skill and experience).
1) First make a solution of alkali.
Prepare a solution of 400 g of NaOH in 1.2 l of water. This should be done in a bucket standing in a basin of water and ice, for it is heated terribly. And better under the air or in the air. The alkali will dissolve, the solution will cool.
2) Preparatory moments
- Ice water is poured into a large basin to cool the impending reaction.
- Preparing a bucket to drain
- The sieve should be at hand!
3) Preparation of a mixture of a solution of FNP with acetic acid
In a glass, FNP is dissolved in IPA in a ratio of 1 g / 10 ml. those. 50g of FNP is dissolved in 500 ml of IPA (sometimes to dissolve propene it is necessary to slightly warm the glass on the tile and ceiling the crystals with a stick), 175 ml of onion or 250 ml of essence are added.
"DO NOT RINSE AMALGAM"
4) Aluminum amalgamation and restoration of PNP
In a 10 liter flask, 75g of crushed aluminum foil (you can use a grinder) are poured, 3 liters of water (turning the flask over will be uncomfortable, and this is putting it mildly, it is easy only in theory), 50 ml of mercury nitrate solution is added (described above). Shake the mixture intensively. For the quickest amalgamation, the flask should be plugged with a cork and shaken VERTICAL (i.e. not so that the contents are mixed in a circle, but up and down). The process can take from 3 to 10 minutes. WELL TO MAKE AMALGAM YOU LEARN ONLY WITH EXPERIENCE. THEREFORE, I RECOMMEND AGAIN TO START WITH SMALL SCALE EXPERIENCES. If you take hot water - foil is amalgamated very quickly, but this is for experienced cooks!
After that, as the foil almost all emerges, loses its luster, and the liquid in the flask becomes dark, all the liquid from the flask is drained through a sieve in the glass, so that the foil remains in the flask. For convenience, it is recommended to take a convex kitchen sieve and attach it to the neck of the flask with a bulge inward (we won’t lose foil). After draining the water ( DO NOT RINSE AMALGAM .
50% of the probability that you will lose everything, I can give you exactly, and "mercury in the final product will NOT fall, all nitrate residues will pass into insoluble oxide during alkalization", I’m keeping silent that the mercury itself will not fall into The top layer under no circumstances )) of course, trace amounts (individual mercury ions) will get into the hair dryer, but this is only interesting for experts who will withdraw it from drug addicts and figure out the method of preparation)) should not be poisoned by mercury when consuming amphetamine) IMMEDIATELY fill1\3 FNP solution with acetic acid (you can half, but note that the reaction warms very much, if you did everything right, be careful at the first), warming up begins - the reaction is underway The flask is put on the reflux refrigerator.
The reaction is carried out at the highest possible temperature, but so that white steam does not roll out from the refrigerator. As soon as the mixture overheats violently - the flask is immersed in a basin of water. As soon as the first heating wave goes down, we add another FNP solution with acid. Everything is done in 2-3 bay. With experience, the entire intensive stage will take you 10-15 minutes.
, no more. It is important - as soon as the RM ceases to be heated VERY STRONGLY - remove the flask from cooling. As soon as the reaction went into decline, put the flask on the table, pour another 250 ml of IPA and carefully mix everything up. We leave for 20-60 minutes so that everything will react (when we scale under the prom. Scale, leaving one reaction complete, set the next one in the other flask).
5) Acid-alkaline extraction.
Remove the reverse fridge and begin to pour in a solution of alkali. Will bask strongly. Stir intensively. Cool, only if completely boils. We will not lose a lot of amphetamine, but the fact that an extra IPA will fly away is not so bad. When all the alkaline solution is added, the mixture continues to stir vigorously. It will start to cool. Add 1250 ml of petroleum ether, thoroughly mix the mixture for 5-10 minutes. It is very important to mix well - it is necessary that the entire base of amphetamine is transferred to a solvent. Pour the mixture into a separatory funnel, let standAfter that we merge the bottom layer. Collected top pour into a glass or flask (volume 5l), add water in the ratio of 1 to 1 (do not be afraid - the base of amphetamine will not go away in water, but extra alkali is necessary) and mix well for several minutes. Then again collect the top layer. It is advisable to let him stand in the freezer - generally perfect. If something settles, filter on it. 700 ml of isopropyl alcohol is added to the collected liquid, a solution of 5.2 ml is prepared in a glass (calculated on a maximum yield of 40g) of sulfuric acid in 50ml of isopropylacetate.
The solution is added slowly. Amphetamine sulfate falls out. I recommend to add half the solution, drain off the product and then acidify the filtrate. ATTENTION - if you add acid, the product will "disappear" (dissolve) - but this is not a reason for panic A simple method is recommended to insure yourself against this. 10% of the unoxidized upper layer is poured into a separate cup and adheres to the "emergency". the remaining 90% acidic solution of sulfuric acid in IPS, adding it slowly. If there is a "perekotsionation" - immediately add the same 10% of the unoxidized upper layer - everything will fall back.
You will also learn with experience to acidify and clearly upset the entire output for 1 reception. With proper adherence to all recommendations, you will receive approximately 35 grams of amphetamine sulphate (the amount of sulfuric acid is 1.3 ml per 10g precipitation). The precipitate is filtered and dried, everything is clear.
The ethyl acetate method (easier and faster in my opinion)
1) Prepare the alkali solution in the same way as above.
2) 50g of PNP dissolved in a liter of ethyl acetate. 175 ml of glacial acetic acid or 250 ml of acetic essence are added.
3) Amalgam is prepared in the same way in a 10 liter flask with the same proportions. Water is poured, the FOURTH of the FNP solution is poured with an acid. WHEN USING ETHYL ACETATE AS A SOLVENT, THE REACTION WILL BE MORE STRONG - BE CAREFUL. The principle of the reaction is the same - we conduct it at the limit of heating, with a reflux condenser, but periodically cool the flask - the reaction mixture should not leave above the middle of the flask. INTENSIVE MOVES.Severe overheating lasts 2-3 minutes, then you can add another quarter of the solution of FNP with acid, then all the rest. The reaction is fast, it can take as little as 10 minutes. As soon as the reaction mixture stops trying to fly out of the flask )), stop cooling, pour another liter of ethyl acetate, mix. At this point, the heating will resume but not so much. Leave until terminated.
4) Acid-alkaline extraction
We conduct alkalization, but this time we try to cool more strongly in order to avoid loss of solvent. After adding all the alkaline solution, pour another 450 ml of ethyl acetate. ATTENTION - IF YOUR LAYERS ALREADY MIX OUT, DO NOT PANIC - ADD ~ 50ml of water, stir, and everything will return to its place. Layers are divided, collect the top. We strip it in half on a tile.
Then put in the freezer (-20 degrees) for a long time. During this time, you can start doing the following reactions. When the collected top layer is frozen, we filter it from all the outsider, if it is, prepare a solution of 5.2 ml of sulfuric acid in 50 ml of ethyl acetate and sour it as well and collect the product.
SCALING.
Suppose we have 10 flasks of 10 liters each.
We act as follows. We prepare a solution of 4 kg of alkali in 12l of water or 10 servings of 400g each in 1.2l (in practice, the second is simpler, the heating is very strong, it is convenient to entrust this work to an assistant). 10 servings of a solution of propene with the addition of glacial acetic acid (or essence) (proportions above). Next, in all 10 flasks we fall asleep 75 g of foil and pour water. After that, we amalgamate the foil in the first flask (by adding 50 ml of mercury nitrate solution), pour out the liquid, conduct the reaction by infusing the solution of propene with acid.
As soon as the reaction can not be cooled (the entire solution of propene with acid is added and 5 minutes have passed), leave this reaction alone, amalgamate the foil in the next flask, drain the liquid, pour in phenylnitropropene with acid, control the rapid phase, proceed to the next flask. And so all 10. Here, all the reactions ended. I do not recommend to merge everything into one barrel and there to alkaline due to the extreme inconvenience of collecting the upper layer in consequence.
Therefore, in each flask we pour the appropriate portion of the alkaline solution, the indicated amounts of solvents (as described above in the methods with petroleum ether or ethyl acetate) and finish the alkalization. We collect the top layer from all flasks in one capacity. If we used petroleum ether, mix the collected liquid with 1 to 1 water. Stir for 10 minutes, separate the top and put in the freezer.If with ethyl acetate - just put in the freezer. Then we prepare, respectively, a solution of 52 ml of sulfuric acid in IPS or ethyl acetate, sour, we collect the product. If you work together, it is very convenient if by the time you pour the FPN with acid into the 5th and 6th flask, and the reaction mixture in the 1st or 2nd flask has already responded and cooled for a long time, your partner will start to alkaline. Those. will go "for you." Line production.The process in 10 flasks with the experience will take several hours and will yield approximately 350 g of the finished product.
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Not my work, trancelated from russian.
(Use google trancelate for desired Language)
"P2NP Russian Methods."
Main Points
1. Do not rinse aliminium, this makes it impossible to melt the aluminium.
2. Reaction Mixtue Should be grey, not white or Pink, deliberate lies by law enforcement.
3. Sodium Hydroxide is essential. Sodium Bicarbonate will not give you anything more than weak cocaine effect, a drug for assholes.
"The most widely used reaction is the synthesis of amphetamine from phenylacetone. It is distinguished by the fact that the synthesis is easily scaled to large volumes of loading, at least 100 kg, and to obtain a pure product at the output. But unfortunately in the Russian Federation the main source component - phenylacetone, is on the lists of narcotic substances, so its purchase is impossible due to its illegal status. All companies that are engaged in the production and marketing of phenylacetone have stopped this activity with the release of the ban."
Nowadays, the most common method of synthesis is the condensation of benzaldehyde with nitroethane in the presence of a catalyst to form 1-phenyl-2-nitropropene, which is then reduced by mercury-aluminum amalgam.
In 2014, nitroethane, benzaldehyde and 1-phenyl-2-nitropropene were added to table 1 of the list of precursors, which significantly complicated the purchase of source codes.
Before the ban, the main source could be bought at a price of 5k per kg of nitroethane and 2k per kg of benzaldehyde. From the bookmark of 1 kg of BA and 1 kg of NE, it turned out to be slightly more than 1 kg of 1-phenyl-2-nitropropene, which, taking into account the catalyst (cyclohexylamine, butylamine or ammonium acetate) and isopropyl alcohol, was released at a cost of 8-9 thousand rubles for cleaning. In this scenario, the final cost of the finished product was 18 000 rubles.
Currently, it is rather difficult to buy source codes for phenylnitropropene, therefore we offer the option of purchasing ready-made PNP in solution, or its legal counterparts, such as phenylnitropropane.
The price for 1kg on the Internet varies from 35k to 50k, respectively, when buying in bulk additional discounts.
In addition to the main source, we will need other reagents. To load 1kg of FNP with an average cost of 40k you need:
5 kg of acetic acid 170r per kg
10l of isopropyl alcohol 150r per liter when buying from 10l
A few grams of mercury salt, which is obtained from metallic mercury from thermometers and nitric acid (200r per liter), thermometers 1.5k
1.2 kg of chopped aluminum foil (60r per roll, 17 rolls)
3 kg of sodium alkali at 130p per kg
100ml of sulfuric acid at 100r per kg
2l acetone 200r per kg
Given the average yield of 70% (without additional manipulations to increase output), the average cost of amphetamine with this method of synthesis is 65,000 rubles (slightly more than $ 1,000)
The price review was conducted in October 2015.
In addition to chemical reagents, we need the simplest equipment, laboratory glass and consumables:
Vacuum pump with 5l Bunsen flask and Buchner funnel - for filtering and washing the finished salt. (8000r per set)
"This kit will help to collect in any chemical store."
Laboratory or kitchen scales (preferably with a calibration weight)
Flat-bottomed 6l flasks with 45 - 4-5 pieces (3000r per pc)
Reverse ball refrigerators loop 45 - 4-5 pieces (2000r per piece)
Basins for cooling flasks during recovery (reaction with a large amount of heat that needs to be kept) (500r per pc)
Different volume laboratory glasses, in the sizes and forms convenient for the cooker. (all glasses can be bought for 3000r)
Alkali Bucket (1000r)
Plastic barrel into which the amalgam held by the conveyor belt will merge (3000)
Latex gloves (200r per pack)
Gauze, or a sieve for draining mercury solution (100r)
Litmus test strips (200r per pack)
Shredder paper shredder (4000r)
Trays for drying the finished product (200r apiece)
20 vat syringes without elastic at the end of the piston (20p per pc)
Desalting Buchner funnel filters (white ribbon) (250r per pack)
To protect clothes a bathrobe (500 rubles) or a painting suit.
Mask with goggles for eye protection and breathing (3000) (3M Mask for Mercury Vavours, Filters should be square pink)
In total, we need about 50,000 rubles to equip the laboratory with glass and equipment.
Additional spending on consumables 1000r
Chemical reagents, equipment and consumables can be purchased at retailers chemical reagents.
All stores are controlled by the authorities, so everything in one place is not worth buying.
Anonymously, but at more expensive prices, you can buy on the forums from Chembro and Mechanics.
A small digression. In this article, we look at the synthesis method in a schematic way. For those who do not have experience assembling amphetamine, you must first get your hand on small quantities, and only then to plan the scaling of the synthesis.
For the first “call to brew”, we recommend that you contact ChemBro or Mechanic’s stores to purchase the assembled “Lego” kit and get technical advice on assembly.
Preparation of the room.
For the work we need a suitable place. The summer cottage is ideal, but you can consider options for placing in the industrial zone, or in the garage. Due to the large odor emission, the apartment is definitely not suitable. There will be enough 20 square square for us, but you can also have a larger area. The presence of electricity is not necessary, but desirable. It is important that the room is well ventilated (windows, or the presence of hoods).During the work we need a fairly large amount of water.
If there is no plumbing and sewage in the room, you will have to bring water and take away waste (for example, if you work in a garage). As a separate article, we will look at cooking in different types of premises in detail, tell you how to equip the space, arrange the equipment, do the drying, whom to arrange, how to preserve anonymity, disguise work and smells.
After you have mastered the laboratory synthesis in small quantities, prepared the premises for the work, purchased the necessary raw materials, equipment, glass, consumables, improvised means and chemical protection, you can start working on amphetamine in large quantities. By a large number, we mean the production of 1kg per day. You can work alone, but for safety, convenience, and increasing the speed of the process it is better to work together.
The whole synthesis process can be divided into several stages:
training
recovery
alkaline
⁃sour
drying and packaging.
During preparation, you need to bring all the reagents and equipment, look around for the presence of pale, cut the foil in advance with a paper shredder (you can immediately hang them in bags), prepare mercury nitrate.
Recovery.
To get 1kg of ready-made amphetamine, we need to supply 1400g of phenylnitpropene. Download all the weight in one tab can not be due to a complex reaction that does not scale well. Therefore, this process is broken down into many, many small tabs, for example, 50g in 6 l flasks. In general, we will need to put 28 flasks (1400g of propene), each of which will take about 40 minutes. Who has enough experience, can increase the working volume of flasks to 10 liters with a load of 70-100gr source. If you work together, you can immediately put 2-3 flasks, which will significantly speed up the process.
The process itself: we take a 6 l flask, pour 60 g of chopped foil into it, pour water over it so that it covers the entire foil and add a pinch of mercury salt. If you have mastered the synthesis in small quantities, you should be well aware of the signs of the finished amalgam. While it is infused, it is necessary to prepare a solution of 50g of PNP + 500ml IPA + 250ml of glacial acetic acid in a laboratory glass.The solution can be slightly heated to dissolve FNP. When the amalgam is ready, we pour out an aqueous solution of mercury salt (for convenience we use a sieve), then add half of the prepared solution of FNP + IPA + LUK to the flask with a fake and close with a reflux condenser (before each new reaction, cold water should be poured into the jacket of the refrigerator, and the nipples should be closed) hose clamps, clamped at the ends, or in the presence of running water, connect a full circulation. These measures will help to avoid excessive evaporation of the IPSa during a violent reaction).Immediately after the bay, a violent exothermic reaction begins (with a large amount of heat). To prevent overheating, the reaction mass should be cooled in a previously prepared basin of water. As soon as the reaction starts to decline, pour the half of the FNP solution remaining in the glass and wait for the reaction to complete. Those who have enough experience and believe in themselves, can immediately pour the entire solution of PNP. In this case there will be a more violent reaction that needs to be carefully controlled. Upon completion of the reaction, which is determined by the attenuation of the process and the dissolution of the foil, the entire reaction mass is poured into a 100 liter drum.
This is the hardest part of the process. Conveyor method need to rotate 28 syntheses of 50g. You can take a smaller amount, it all depends on the needs, for example, to reduce the planned output by half, that is, by 500g of the finished amphetamine. Then we will need to put 700gr source.
Alkalization
Alkalization is the simplest process in all synthesis. Alkaline we will be in a 100l barrel previously prepared cold alkali solution. The solution is prepared as follows: take a bucket, pour 4.5 kg of alkali into it, fill it with water until the alkali dissolves, usually 7l is enough. Immediately begins abundant heat. We wait until it cools, stirring occasionally. Cooling may take up to 2 hours.
Before alkalization, unreacted aluminum should be collected in the barrel with the reaction mass. This can be done by filtering the entire reaction mass through gauze or a sieve. If this is not done, the foil will react with alkali, additionally heating the mixture and releasing by-products.
Then in small portions gradually pour cold alkali into the RM. Warming up and subsequent separation into layers will begin. We need to carefully collect the entire top layer - this is ready-made amphetamine as a base, a solution in alcohol.
The bottom layer is sludge, in which 10% -20% of the product remains, which can be obtained by extraction. Extract with solvent, evaporate and combine with base oil. Pour the sludge, it is no longer needed.
Souring.
Probably the most interesting and important process. It is most convenient to sour in a wide laboratory glass of 500-1000ml. In a 250ml glass we prepare a solution of sulfuric acid in acetone (for 1ml of sulfur, 15ml of acetone). We pour a quarter of a glass with the base of phenamine and gradually, in small portions, from a 20 ml syringe, add our solution of sulfuric acid in acetone. Amphetamine sulphate flakes will start to fall.Sour gently to pH 5.5. If the mixture thickens strongly, then dilute it with a small amount of acetone so that there is no local over-acidification. If you peroxide, you can lose the whole product. So we have to acidify all the oil. Next, you need to thoroughly rinse the mass with acetone and press on the vacuum filtration system.
Drying & Packaging.
The washed and pressed product is unloaded on trays, dried at room temperature until completely dry. We weigh the dry, crumbly product and pack it in the necessary packing. We carry out cleaning of the room, we take out garbage.
We have dismantled the most popular at the moment the synthesis of amphetamine. At first glance, the process looks confused, with its difficulties. But with the proper approach and experience, everything goes coasting without any serious problems. A very big disadvantage of this method is the impossibility of scaling the reduction reaction. But even with the work in 6l-10l flasks, you can achieve monthly output of 15-30 kg in two cooks.
There are other ways to obtain this wonderful product, which we will keep in reserve in case of banning or withdrawing phenylnitropropene in solution and its analogues. Therefore, fans will accelerate the classics do not worry, for a long time you can pamper yourself with amphetamine.
SCALE PRODUCTION OF AMPHETAMINE
1 option proportions:
1 kg Phenylnitropropene (FNP) ~ 30000 - 50000r
3.5 kg Icy Acetic Acid (or 5kg 70% Acetic Essence) ~ 700-1000р
1.5kg Aluminum Foil (I recommend 11 microns thickness) ~ 1250r
30l Isopropyl Alcohol - less than 5000r
25 liters liters Petroleum ~ 4500r
Approximately 100ml Sulfuric Acid - less than 200r
8kg NaOH (Sodium Hydroxide, Alkali) - less than 1000r
Dry Mercury Nitrate or Mercury Nitrate Solution, obtained from 50 degree pharmacy and 100 ml of nitric acid (68%, density 1.4), followed by neutralization of excess acid drinking soda ~ 3000r
----------------------------------------------------------------------------------------------------------------------
TOTAL 45000-65000r = yield approximately 700g of pure amphetamine sulfate (cost 64000-93000 / 1kg)
2 variant proportions (I personally recommend it):
1kg Phenylnitropropene (FNP) - 30000-50000r
3.5 kg Icy Acetic Acid (or 5kg 70% Acetic Essence) ~ 700-1000р
1.5kg Aluminum Foil (I recommend 11 microns thickness) ~ 1250r
50l Ethyl acetate ~ 5000r
Approximately 100ml Sulfuric Acid - less than 200r
8kg NaOH (Sodium Hydroxide, Alkali) - less than 1000r
Dry Mercury Nitrate or Mercury Nitrate Solution, obtained from 50 degree pharmacy and 100 ml of nitric acid (68%, density 1.4), followed by neutralization of excess acid drinking soda ~ 3000r
TOTAL: 31000 - 61450 = Approximately 700g yield of amphetamine sulfate (cost 44300 - 87800r / kg)
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Mercury nitrate, cooking. (Skip if you have Mercury (ii) chloride)
Let's look at the wholesale manufacture of mercury nitrate for mass production of amphetamine.
In fact, to get mercury from thermometers is not dangerous and not scary, it is done elementary. First we put on gloves Option 1. A 2-liter dry glass is taken, narrow, placed on a hard surface (so as not to crack the glass), after which the thermometers are thrown tip-down. They naturally break, mercury flows out, you can knock a broken thermometer on the walls of the glass so that everything flows out, after which the thermometer is thrown into a prepared bucket next to it. The procedure is repeated 50 times (50 thermometers are broken into a glass).Next on the balcony \ in the open \ under the hood is installed stove. On the tile we put a glass with the extracted mercury, the tile is not included yet. Fill in a glass with 100 ml of nitric acid (density 1.4). The reaction begins with the release of brown vapor. Periodically stir everything with a glass rod, chasing balls of mercury. As soon as the reaction diminishes, we turn on the electric stove for a small power (Pts cannot be heated very much). The reaction to resume, mercury will gradually dissolve. If the temperature of PM is more than 50 degrees and the reaction does not go, we can add more nitric acid from the syringe, but in practice you never have to add more than 50 ml to 50 thermometers (i.e. + 1 ml per thermometer), most likely in such cases 5-10 ml will be enough. But, most likely, it will not be necessary to add it at all. The reaction is carried out until complete dissolution of mercury. After that, dilute the mixture with about 300 ml of water. Next, you need to neutralize the acid residues. To do this, in a glass, a LITTLE BIT (you can take a quarter of a teaspoon), add baking soda with vigorous stirring. Mixture
will foam strongly (carbon dioxide is released), soda will dissolve. Adding soda in small portions, continue until, after adding the next portion, an insoluble yellow color precipitate forms in the mixture. As soon as this happens, we collect nitric acid in the syringe and add it with DROPS with vigorous stirring until the precipitate dissolves. Now the mercury nitrate solution is neutralized. You may ask why this is necessary and why.
nitric acid cannot be infused with the calculation of "10 cubic meters per thermometer", as others advise - because excess acid in mercury nitrate solution (if you are not going to pour this nitrate solution into a crystallizer and get mercury nitrate in a dry form) can play a VERY cruel joke with you when preparing amalgam. Believe me, when it burns - it is very unpleasant, and if a piece of such foil comes into your hands - no gloves will help with severe burns).So, we have neutralized the mercury nitrate solution, now we dilute it with water in a glass to the 1 liter mark. IT IS VERY CONVENIENT. Since a liter of this solution will be consumed when recovering 1 kg of propene. Those. if we take a load of 50 g of PNP, then 75 g of foil will be processed to be used for its recovery, it will take 50 ml of this solution of mercury nitrate. Agree, it is convenient.
Option 2. Everything is the same as in option 1, just take a two-liter flask, lower the thermometer with the tip into the neck and have a snack with pliers, do it all with all the 50th thermometers, just pour nitric acid 100ml, heat it, dissolve the mercury, dilute it with water , neutralize with soda, bring the volume of the solution to 1 liter.
---------------------------------------------------------------------------------------------------------------
Phenylnitropropene reduction 50 gram Batch! (amphetamine synthesis).
Method with isopropyl alcohol (IPA) and petroleum ether
Synthesis of 50 gram loading. Of course, cooks need to practice their skills at a load of 5-10 g of FNP in a 2 liter flask (you can easily count the proportions, the main truth is to start small. The synthesis is simple, but it requires skill and experience).
1) First make a solution of alkali.
Prepare a solution of 400 g of NaOH in 1.2 l of water. This should be done in a bucket standing in a basin of water and ice, for it is heated terribly. And better under the air or in the air. The alkali will dissolve, the solution will cool.
2) Preparatory moments
- Ice water is poured into a large basin to cool the impending reaction.
- Preparing a bucket to drain
- The sieve should be at hand!
3) Preparation of a mixture of a solution of FNP with acetic acid
In a glass, FNP is dissolved in IPA in a ratio of 1 g / 10 ml. those. 50g of FNP is dissolved in 500 ml of IPA (sometimes to dissolve propene it is necessary to slightly warm the glass on the tile and ceiling the crystals with a stick), 175 ml of onion or 250 ml of essence are added.
"DO NOT RINSE AMALGAM"
4) Aluminum amalgamation and restoration of PNP
In a 10 liter flask, 75g of crushed aluminum foil (you can use a grinder) are poured, 3 liters of water (turning the flask over will be uncomfortable, and this is putting it mildly, it is easy only in theory), 50 ml of mercury nitrate solution is added (described above). Shake the mixture intensively. For the quickest amalgamation, the flask should be plugged with a cork and shaken VERTICAL (i.e. not so that the contents are mixed in a circle, but up and down). The process can take from 3 to 10 minutes. WELL TO MAKE AMALGAM YOU LEARN ONLY WITH EXPERIENCE. THEREFORE, I RECOMMEND AGAIN TO START WITH SMALL SCALE EXPERIENCES. If you take hot water - foil is amalgamated very quickly, but this is for experienced cooks!
After that, as the foil almost all emerges, loses its luster, and the liquid in the flask becomes dark, all the liquid from the flask is drained through a sieve in the glass, so that the foil remains in the flask. For convenience, it is recommended to take a convex kitchen sieve and attach it to the neck of the flask with a bulge inward (we won’t lose foil). After draining the water ( DO NOT RINSE AMALGAM .
50% of the probability that you will lose everything, I can give you exactly, and "mercury in the final product will NOT fall, all nitrate residues will pass into insoluble oxide during alkalization", I’m keeping silent that the mercury itself will not fall into The top layer under no circumstances )) of course, trace amounts (individual mercury ions) will get into the hair dryer, but this is only interesting for experts who will withdraw it from drug addicts and figure out the method of preparation)) should not be poisoned by mercury when consuming amphetamine) IMMEDIATELY fill1\3 FNP solution with acetic acid (you can half, but note that the reaction warms very much, if you did everything right, be careful at the first), warming up begins - the reaction is underway The flask is put on the reflux refrigerator.
The reaction is carried out at the highest possible temperature, but so that white steam does not roll out from the refrigerator. As soon as the mixture overheats violently - the flask is immersed in a basin of water. As soon as the first heating wave goes down, we add another FNP solution with acid. Everything is done in 2-3 bay. With experience, the entire intensive stage will take you 10-15 minutes.
, no more. It is important - as soon as the RM ceases to be heated VERY STRONGLY - remove the flask from cooling. As soon as the reaction went into decline, put the flask on the table, pour another 250 ml of IPA and carefully mix everything up. We leave for 20-60 minutes so that everything will react (when we scale under the prom. Scale, leaving one reaction complete, set the next one in the other flask).
5) Acid-alkaline extraction.
Remove the reverse fridge and begin to pour in a solution of alkali. Will bask strongly. Stir intensively. Cool, only if completely boils. We will not lose a lot of amphetamine, but the fact that an extra IPA will fly away is not so bad. When all the alkaline solution is added, the mixture continues to stir vigorously. It will start to cool. Add 1250 ml of petroleum ether, thoroughly mix the mixture for 5-10 minutes. It is very important to mix well - it is necessary that the entire base of amphetamine is transferred to a solvent. Pour the mixture into a separatory funnel, let standAfter that we merge the bottom layer. Collected top pour into a glass or flask (volume 5l), add water in the ratio of 1 to 1 (do not be afraid - the base of amphetamine will not go away in water, but extra alkali is necessary) and mix well for several minutes. Then again collect the top layer. It is advisable to let him stand in the freezer - generally perfect. If something settles, filter on it. 700 ml of isopropyl alcohol is added to the collected liquid, a solution of 5.2 ml is prepared in a glass (calculated on a maximum yield of 40g) of sulfuric acid in 50ml of isopropylacetate.
The solution is added slowly. Amphetamine sulfate falls out. I recommend to add half the solution, drain off the product and then acidify the filtrate. ATTENTION - if you add acid, the product will "disappear" (dissolve) - but this is not a reason for panic A simple method is recommended to insure yourself against this. 10% of the unoxidized upper layer is poured into a separate cup and adheres to the "emergency". the remaining 90% acidic solution of sulfuric acid in IPS, adding it slowly. If there is a "perekotsionation" - immediately add the same 10% of the unoxidized upper layer - everything will fall back.
You will also learn with experience to acidify and clearly upset the entire output for 1 reception. With proper adherence to all recommendations, you will receive approximately 35 grams of amphetamine sulphate (the amount of sulfuric acid is 1.3 ml per 10g precipitation). The precipitate is filtered and dried, everything is clear.
The ethyl acetate method (easier and faster in my opinion)
1) Prepare the alkali solution in the same way as above.
2) 50g of PNP dissolved in a liter of ethyl acetate. 175 ml of glacial acetic acid or 250 ml of acetic essence are added.
3) Amalgam is prepared in the same way in a 10 liter flask with the same proportions. Water is poured, the FOURTH of the FNP solution is poured with an acid. WHEN USING ETHYL ACETATE AS A SOLVENT, THE REACTION WILL BE MORE STRONG - BE CAREFUL. The principle of the reaction is the same - we conduct it at the limit of heating, with a reflux condenser, but periodically cool the flask - the reaction mixture should not leave above the middle of the flask. INTENSIVE MOVES.Severe overheating lasts 2-3 minutes, then you can add another quarter of the solution of FNP with acid, then all the rest. The reaction is fast, it can take as little as 10 minutes. As soon as the reaction mixture stops trying to fly out of the flask )), stop cooling, pour another liter of ethyl acetate, mix. At this point, the heating will resume but not so much. Leave until terminated.
4) Acid-alkaline extraction
We conduct alkalization, but this time we try to cool more strongly in order to avoid loss of solvent. After adding all the alkaline solution, pour another 450 ml of ethyl acetate. ATTENTION - IF YOUR LAYERS ALREADY MIX OUT, DO NOT PANIC - ADD ~ 50ml of water, stir, and everything will return to its place. Layers are divided, collect the top. We strip it in half on a tile.
Then put in the freezer (-20 degrees) for a long time. During this time, you can start doing the following reactions. When the collected top layer is frozen, we filter it from all the outsider, if it is, prepare a solution of 5.2 ml of sulfuric acid in 50 ml of ethyl acetate and sour it as well and collect the product.
SCALING.
Suppose we have 10 flasks of 10 liters each.
We act as follows. We prepare a solution of 4 kg of alkali in 12l of water or 10 servings of 400g each in 1.2l (in practice, the second is simpler, the heating is very strong, it is convenient to entrust this work to an assistant). 10 servings of a solution of propene with the addition of glacial acetic acid (or essence) (proportions above). Next, in all 10 flasks we fall asleep 75 g of foil and pour water. After that, we amalgamate the foil in the first flask (by adding 50 ml of mercury nitrate solution), pour out the liquid, conduct the reaction by infusing the solution of propene with acid.
As soon as the reaction can not be cooled (the entire solution of propene with acid is added and 5 minutes have passed), leave this reaction alone, amalgamate the foil in the next flask, drain the liquid, pour in phenylnitropropene with acid, control the rapid phase, proceed to the next flask. And so all 10. Here, all the reactions ended. I do not recommend to merge everything into one barrel and there to alkaline due to the extreme inconvenience of collecting the upper layer in consequence.
Therefore, in each flask we pour the appropriate portion of the alkaline solution, the indicated amounts of solvents (as described above in the methods with petroleum ether or ethyl acetate) and finish the alkalization. We collect the top layer from all flasks in one capacity. If we used petroleum ether, mix the collected liquid with 1 to 1 water. Stir for 10 minutes, separate the top and put in the freezer.If with ethyl acetate - just put in the freezer. Then we prepare, respectively, a solution of 52 ml of sulfuric acid in IPS or ethyl acetate, sour, we collect the product. If you work together, it is very convenient if by the time you pour the FPN with acid into the 5th and 6th flask, and the reaction mixture in the 1st or 2nd flask has already responded and cooled for a long time, your partner will start to alkaline. Those. will go "for you." Line production.The process in 10 flasks with the experience will take several hours and will yield approximately 350 g of the finished product.
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# 2
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
Mevzy mnie jeszcze pytanie bo cos przeoczylem. Jak wykonac prawidlowo amalgamat aluminium. Czy cos zle robie?
-gruba folia aluminiowa pocieta w kwadraty 8 gramow
-wrzucona do 200ml wody destylowanej
-wsypuję 25g hgcl2 (II)
-mieszam ( jak dlugo mieszac? ) --
-czekam 20min
-I teraz to czego pojac nie zrozumialem. WYLEWAM ZAWARTOSC I MYJE 3 RAZY WODA BLOCZKI ALUMINIUM? Co nadtepnie z nimi robie.
Prosze o wyczerpujaca odpowiedz. Wszystkie informacje w celavh edukacyjnych teoretycznych
-gruba folia aluminiowa pocieta w kwadraty 8 gramow
-wrzucona do 200ml wody destylowanej
-wsypuję 25g hgcl2 (II)
-mieszam ( jak dlugo mieszac? ) --
-czekam 20min
-I teraz to czego pojac nie zrozumialem. WYLEWAM ZAWARTOSC I MYJE 3 RAZY WODA BLOCZKI ALUMINIUM? Co nadtepnie z nimi robie.
Prosze o wyczerpujaca odpowiedz. Wszystkie informacje w celavh edukacyjnych teoretycznych
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
Znajomy chemik kiedyś zrobił mi p2np lecz kontakt się urwał. Da ktoś namiary na priv?
Synteza siarczanu amfetaminy z fenylonitropropenu(P2NP)
jak ktoś ma mieć namiary na Twojego chemika
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NIE porównuj sklepów w działach partnerskich. Nie pytaj tam o produkty, których sklepy nie oferują. Są od tego inne działy!
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Poradnik dodawania zdjęć | How to add photos?
Rangi na forum | Ranks on forum
Awans na pełnoprawnego użytkownika | Promotion to a full-fledged user
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