Jednogarnkowa synteza amfetaminy z P2NP z NaBH4/CuCl2 (skala 1 kg)

SelfExper1menter

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Witam wszystkich. Próbowałem zrobić amfetaminę według tego przepisu na małą skalę, ale nie udało mi się. Wszystko wydawało się w porządku, po wysuszeniu mój produkt wyglądał jak biały proszek z odcieniem czerwieni. Gdyby to był siarczan amfetaminy (który próbowałem zrobić), wydajność wynosiłaby 84%. Problem w tym, że to nie jest amfetamina.

Efekty fizjologiczne
Próbowałem 20-30 mg, zdecydowanie było pobudzenie, ale także spowodowało gorączkę i, najwyraźniej, spadek odporności: za każdym razem, gdy brałem to przez kilka dni z rzędu, zachorowałem na infekcje dróg oddechowych (za pierwszym razem myślałem, że to przypadek). Inna osoba, która go zażywała, nie doświadczyła żadnej stymulacji przy dawce do 90 mg, jedynie pewną suchość w ustach. Żadne z nas nie ma tolerancji na stymulanty.

Testy chemiczne
1 g proszku całkowicie rozpuszcza się w 10 ml H2O.
Kiedy dodałem nadmiar roztworu NaOH do odmierzonej masy proszku w probówce, otrzymałem w przybliżeniu odpowiednią objętość wolnej bazy o zapachu amoniaku. Oddzieliłem warstwę wolnej zasady, osuszyłem ją za pomocą CaCl2 i spróbowałem zmiareczkować kwasem. W rezultacie zmierzyłem masę molową wolnej zasady na około 171 (a dla amfetaminy jest to 135). Chociaż moje pomiary nie były zbyt dokładne, różnica jest nadal zbyt duża, aby można ją było wyjaśnić samymi błędami pomiarowymi.

Moje odstępstwa od procedury

1) Podczas dodawania P2NP zdałem sobie sprawę, że zajmie to wiele godzin, więc zniecierpliwiłem się i zanurzyłem kolbę reakcyjną w łaźni wodnej o temperaturze pokojowej. Potem udało mi się dodać P2NP prawie w całości na raz, a temperatura mieszaniny nie przekroczyła 40-50°C.
2) Postępowałem zgodnie z filmem, więc nie odparowałem IPA i dodałem stężony kwas siarkowy bezpośrednio do warstwy IPA/wolnej bazy.
3) Nie miałem w tej chwili acetonu, więc nie dodałem go przed zakwaszeniem i przemyłem przefiltrowaną pastę "siarczanu amfetaminy" za pomocą IPA.
4) IPA jest mniej lotny niż aceton, więc musiałem umieścić mój osad w piekarniku na kilka godzin, aby wysuszyć go do stałej wagi. Temperatura w piekarniku nie przekraczała 80°C.

Najważniejsze pytanie brzmi: gdzie popełniono błąd? Nie byłbym zaskoczony niską wydajnością lub brakiem produktu, ale uzyskanie dobrej wydajności aminy, która nie jest amfetaminą?
 
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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?
 

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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