Síntese de anfetamina em um único recipiente a partir de P2NP com NaBH4/CuCl2 (escala de 1kg)

SelfExper1menter

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Olá a todos. Tentei fazer um pouco de anfetamina usando esta receita em pequena escala, mas falhei. Tudo parecia bem, mas depois de secar o meu produto parecia um pó branco com um toque de vermelhidão. Se fosse sulfato de anfetamina (que eu estava a tentar fazer), o rendimento seria de 84%. O problema é que não se trata de anfetamina.

Efeitos fisiológicos
Experimentei 20-30 mg, houve definitivamente estimulação, mas também provocou febre e, aparentemente, uma diminuição da imunidade: das duas vezes que a tomei durante vários dias seguidos, adoeci com infecções respiratórias (da primeira vez pensei que fosse coincidência). Outra pessoa que a tomou não sentiu qualquer estimulação até 90 mg, apenas alguma secura na boca. Nenhum de nós tem tolerância a estimulantes.

Testes químicos
1 g do pó dissolve-se completamente em 10 ml de H2O.
Quando adicionei uma solução de NaOH em excesso a uma massa medida do pó num tubo de ensaio, obtive um volume aproximadamente correto de base livre com cheiro a amoníaco. Separei a camada de base livre, sequei-a com CaCl2 e tentei titulá-la com ácido. Como resultado, medi a massa molar da base livre como sendo cerca de 171 (e para a anfetamina é 135). Embora as minhas medições não tenham sido muito precisas, a diferença é demasiado grande para ser explicada apenas por erros de medição.

Os meus desvios ao procedimento

1) Ao adicionar P2NP, apercebi-me que ia demorar horas, por isso fiquei impaciente e mergulhei o balão de reação num banho de água à temperatura ambiente. Depois disso, consegui adicionar o P2NP quase todo de uma vez, e a temperatura da mistura não ultrapassou 40-50 °С.
2) Eu estava seguindo o vídeo, então eu não evaporei o IPA e adicionei conc. ácido sulfúrico para a camada IPA / freebase diretamente.
3) Eu não tinha acetona no momento, então não a adicionei antes de acidificar e lavei a pasta filtrada de "sulfato de anfetamina" com IPA.
4) O IPA é menos volátil do que a acetona, pelo que tive de colocar o meu precipitado numa estufa durante várias horas para o secar até atingir um peso constante. A temperatura no forno não excedeu 80 ° С.

Então, a grande questão é: onde é que correu mal? Eu não ficaria surpreso com baixo rendimento ou nenhum produto, mas obter um bom rendimento de uma amina que não é anfetamina?
 
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OrgUnikum

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The method as described here lacks all product workup/cleanup and and as such provides a very dirty and unclean Amphetamine, in special as NasBH4 reductions are all not giving very clean product. Purple MDMA and such.
I know the physiological effects like fever like very well and it is just the missing cleaning trust me.
There are several ways to do the workup, from distillation, normal, vacuum or steam of the base or dissolving the sulfate in water and washing this several times with toluene or petrolether or my favorite: 50/50 mix of petrol ether and Ethylacetate. Then evaporate the water and wash the resulting salt with copious amounts of Acetone and petrol ether as last. Already the simple washings give you a consumable product which does not make you sick like the crap which contains borate salts or else.
 

waltjr5858

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Even with the dirtiest amp he would have felt it just fine....guaranteed he got "almost amp" mainly riddled with hydroxylamine. This reaction goes south on people all the time. They have wayyyy too much nabh4 left when it's time to add the copper and with the heat the nanoparticles aggregate and become completely useless as a catalyst....fully useless... and leave semi reduced product. The only way I've been able to get around that is by reducing 1st in methanol/thf to propane then extracting and then using anyone of the zinc/formic acid combos.... for the nitro. Zero Michael addition.
 

Pajmon

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7Larq9OUew
I tried it today, but something must have gone wrong..I followed the instructions exactly, but in the end there is more than there should be. What could have happened? Can anyone give me advice? Can it be cleaned? Thank you for every answer
 

Pajmon

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Please. How do I have a reaction more nabh4? I threw in for 6 hours but still not much nabh4 dissolved. In the end, when I added acid, the whole thing thickened after filtration, a white substance remained, but I suppose it's nabh4.. I followed the instructions I don't know what's wrong.
 

Swirly

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My mescaline guide might help for 1 or 2 mol amounts. Possibly up to 500 g+ in a 20 L reaction vessel.

The same procedure for P2NP as with Mescaline nitrostyrene, however I do not know if it is more reactive. Have not worked with it.

Take a look here:

Or posted here (if starting from benzaldehyde):
 

pureevil

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My friend and I always cooked amphetamine in the forest.
That is, for synthesis we really only needed 3 construction basins, Phenyl-nitropropene, several boxes of mercury thermometers, hydrochloric acid, gasoline and some special ribbons that show the reaction.

My role was always bring and serve, but we produced this product of 99.8% purity.
We had no competition in Moscow :/
JkXmlJKwSW
R26aY5Ubl3
W3xgS2lksF


we didn't use fucking acetone because it's bad for your health
 
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GhostChemist

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What is the salt of amphetamine present on this photos?
 
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pureevil

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At one point in Russia, they suddenly cut off the liquid propen supply—left a bunch of wannabe cooks totally clueless. Product turned out nasty as hell, colors ranging from sketchy pinks to filthy yellows and straight-up horrifying oranges. But my homie was different—he was one of the few who knew the synthesis inside and out. Back in the day, he cooked pristine pervitin for the whole block, but dude got busted—hit him with a solid 20-year stretch. Luckily there’s a war poppin' off, so he'll probably get tossed onto the front lines and bounce back home early. Then we'll pick right back up where we left off.
 

GhostChemist

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but you say "...3 construction basins, Phenyl-nitropropene, several boxes of mercury thermometers, hydrochloric acid, gasoline and some special ribbons..." and in your list of reagents only hydrochloric acid
 

pureevil

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I can hit him up and get the full cook recipe—it's fuckin' one-of-a-kind.
 

GhostChemist

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in this synthesis using only this reagents "...Phenyl-nitropropene, several boxes of mercury thermometers, hydrochloric acid, gasoline and some special ribbons..." amp sulfate cannot be obtained.

with hydrochloric acid obtain amp hydrochloride
with sulphuric acid obtain amp sulphate
 

G.Patton

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Your reagents list remind different synthesis way (Al/Hg approach). Why did you write this post under NaBH4 method? It's, also, interesting about HCl and sulphate salt.
 

Pajmon

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Lately, I have not been able to get this reaction. I don't know what I'm doing wrong. Before that, I had better results. I always make only a lot of 10 grams, I don't know what I'm doing wrong, maybe someone can help. I have the ratio of substances as in the video, I use a half-liter flask with 3 holes - thermometer, cooler and hole where I put it. I use magnetic stirring. I think that's enough for that amount. In the first phase, my temperature is around 40-50 degrees, every time it starts to drop, I make a match. I tried 2 but also 4 hours with the same result. In the second phase, when I add a small amount, my temperature does not rise, as a result I have maybe half a gram. Before that, I used to have 5-6 grams. After adding H3PO4 drops, the whole thing thickened, now only a little bit is formed. I don't know what I'm doing wrong
 

G.Patton

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Hi. Did you ad CuCl2 and reach this temperature?
 
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Pajmon

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yes, after adding CuCl2, I keep the temperature at 75-80 °C. When I did it before, it worked. I don't know where I'm making a mistake and why the yield is so small.. I'll try a different extraction method, I read somewhere here that it works without acetone
 

Pajmon

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When I finish the first phase the temperature is around 50c. then I add CuCl2 but the temperature doesn't increase by itself I have to heat it up and I think the reaction is going on for a short time I follow it by the formation of bubbles but I don't know if that's right..otherwise everything looks like in the video. it happened to me but when I put a-oil in the freezer ice formed there so I think that in the phase when the hydroxide is added it didn't distribute as it should but I also don't know why..I'll try to buy another IPA, I used it differently than when I did it before. maybe that's the problem.. I'm most angry when I tried it the first time it worked much better
 

G.Patton

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What color of your CuCl2?
>>but when I put a-oil in the freezer ice formed there
On a what step? Was it after acidification on Step 11? It's okay because your acid contains water. What pH have you reached?
 

Pajmon

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The color of CuCl2 is the same as in the video, and I only added a few drops of acid, but there was a lot of ice. I don't know what I'm doing wrong, everything looks good, the temperature has also risen after adding CuCl2, you need to have a higher temperature than I had. A-oil looks good, but I can't get amphetamine... and I'm gradually lowering the pH to 5.
 

G.Patton

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As I see, the problem with acidification procedure. You should reach pH6, not less.

So, you get a-oil, separate it from IPA and did everything like in the method?
 

mile123

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Hello!

I built small version of batch chemical reactor that has 0.01C temperature precision, handle vacuum distillation while stirring, accurately add p2np in small portions using feeder, built from organic chemistry glassware. If you feed it with correct amounts and chemicals, it would produce without putting any additional effort.

I'm looking for a partner, who can get me chemicals in larger quantities, especially nitroethane. Chemical knowledge is also welcomed, since I'm mechanical engineer.
It would take me a lot of effort and energy to get the chemicals while I want to foucus on technology and product.

Send me dm if you are interested.
 
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