Синтез на амфетамин от P2NP с NaBH4/CuCl2 в едно гърне (мащаб 1 kg)

SelfExper1menter

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Здравейте на всички. Опитах се да направя малко амфетамин по тази рецепта в малък мащаб, но не успях. Всичко изглеждаше наред, след като изсъхна, продуктът ми приличаше на бял прах с оттенък на зачервяване. Ако това беше амфетамин сулфат (който се опитвах да направя), добивът щеше да бъде 84%. Проблемът е, че това не е амфетамин.

Физиологични ефекти
Опитах 20-30 mg, определено имаше стимулация, но също така предизвика повишена температура и, очевидно, спад на имунитета: и двата пъти, когато го взех няколко дни подред, се разболях от респираторни инфекции (първия път си помислих, че е съвпадение). Друг човек, който го е приемал, не е изпитал никакво стимулиране от до 90 mg, а само известна сухота в устата. Нито един от нас няма никаква толерантност към стимуланти.

Химическо изследване
1 g от праха се разтваря напълно в 10 ml H2O.
Когато добавих излишен разтвор на NaOH към измерената маса на праха в епруветка, получих приблизително правилен обем свободна основа с мирис на амоняк. Отделих слоя фребаза, изсуших го с CaCl2 и се опитах да го титрувам с киселина. В резултат на това измерих, че моларната маса на фрибазата е около 171 (а за амфетамина е 135). Въпреки че измерванията ми не бяха много точни, разликата все пак е твърде голяма, за да се обясни само с грешки при измерването.

Отклоненията ми от процедурата

1) При добавянето на P2NP разбрах, че ще отнеме часове, затова проявих нетърпение и потопих колбата с реакцията във водна баня със стайна температура. След това успях да добавя P2NP почти наведнъж, а температурата на сместа не надхвърли 40-50 °С.
2) Следвах видеото, така че не изпарих IPA и добавих конц. сярна киселина директно към слоя IPA/замърсител.
3) В момента не разполагах с ацетон, така че не го добавих преди подкиселяването и промих филтрираната паста "амфетамин сулфат" с IPA.
4) IPA е по-малко летлив от ацетона, така че трябваше да сложа утайката си във фурната за няколко часа, за да я изсуша до постоянно тегло. Температурата във фурната не надвишаваше 80 °С.

И така, големият въпрос е къде се обърках? Не бих се изненадал от нисък добив или липса на какъвто и да е продукт, но да получа добър добив на амин, който не е амфетамин?!
 
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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.
 
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