Синтез амфетамина в одном горшке из P2NP с помощью NaBH4/CuCl2 (масштаб 1 кг)

[SelfExper1menter]

Всем привет. Я пытался сделать амфетамин по этому рецепту в небольших масштабах, но потерпел неудачу. Все вроде бы хорошо, но после сушки мой продукт выглядел как белый порошок с оттенком красноты. Если бы это был сульфат амфетамина (который я пытался сделать), то выход составил бы 84%. Проблема в том, что это не амфетамин.

Физиологические эффекты
Я пробовал 20-30 мг, стимуляция определенно была, но также она вызывала жар и, видимо, снижение иммунитета: оба раза, когда я принимал ее несколько дней подряд, я заболевал респираторными инфекциями (в первый раз я подумал, что это совпадение). Другой человек, принимавший его, не испытывал никакой стимуляции от дозы в 90 мг, только некоторую сухость во рту. Ни у кого из нас нет толерантности к стимуляторам.

Химическое тестирование
1 г порошка полностью растворяется в 10 мл H2O.
Когда я добавил избыток раствора NaOH к отмеренной массе порошка в пробирке, получился примерно правильный объем свободной основы с запахом аммиака. Я отделил слой свободного основания, высушил его CaCl2 и попытался титровать кислотой. В результате я измерил молярную массу фребазы, которая составила около 171 (а для амфетамина - 135). Хотя мои измерения не были очень точными, разница все равно слишком велика, чтобы ее можно было объяснить только погрешностями измерений.

Мои отклонения от процедуры
1) При добавлении P2NP я понял, что это займет несколько часов, поэтому я проявил нетерпение и погрузил реакционную колбу в водяную баню комнатной температуры. После этого мне удалось добавить P2NP почти весь сразу, а температура смеси не превышала 40-50 °С.
2) Я следовал видео, поэтому не выпаривал IPA и добавил конц. серную кислоту непосредственно в слой IPA/фрибаза.
3) Ацетона у меня в тот момент не было, поэтому я не стал добавлять его перед подкислением и промыл отфильтрованную пасту "амфетамин сульфат" IPA.
4) IPA менее летуч, чем ацетон, поэтому мне пришлось поместить осадок в духовку на несколько часов, чтобы высушить его до постоянной массы. Температура в духовке не превышала 80 °С.

Итак, главный вопрос - где все пошло не так? Я бы не удивился низкому выходу или полному отсутствию продукта, но получить хороший выход амина, который не является амфетамином?!

 

[OrgUnikum]

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.

 

[w2x3f5]

CaCl2 нельзя использовать с амином
1.на первой стадии нитропропен восстанавливается до нитропропана
2.получали примеси различных солей в составе амфетаминовой пасты

 

[GhostChemist]

Chemical testing
The acid concentration must be precisely known (titration with standart solution of NaOH).
In the titrimetric analysis the concentration must be used only in equivalent concentration or normality or molality.
If one reagent is a weak acid or base and the other is a strong acid or base, the titration curve is irregular and the pH shifts less with small additions of titrant near the equivalence point. Indicators such as Methyl red or Litmus should give more accurate results
This method cannot be applied in this implementation

 

[Ironbender]

I tried this synthesis on a small scale.
It failed completely. In the end I didn't even receive A-Oil.

This was my path:

p2np 10g

IPA/H2O (1:2) IPA 120ml/H2O 60ml (180ml)

NaBH4 17.4g

CuSO4.5H2O 7.9g in 20ml H2O

NaOH 25.6g in 80ml H2O

First water and then IPA were filled into the flask at room temperature and stirred.

NaBH4 was completely filled into the flask and stirred overhead.

p2np was added over a period of 30 min.
The temperature did not rise above 45 degrees.

When all P2NP was in the flask I increased the temperature to 55-58 degrees and refluxed for 40 minutes.

Then CuSO4.5H2O
dropped into the flask. Black copper immediately formed
Somehow the temperature didn't increase.

The RM was heated in a water bath to 78-80 degrees for 30 minutes.

The flask was left at room temperature for 1 hour.

There were 2 layers in the flask, black copper at the bottom. 'Amber cloudy at the top.

There was something slightly yellow in between that couldn't be dissolved.

Then 80 ml of 25% NaOH was added to the RM and a dark amber layer became visible.

It didn't smell like amphetamine base,
it smelled very flowery.
Nothing reminiscent of Amphetamine Oil.

Can someone explain what was wrong?
I followed the small scale instructions from this thread

p2np was from BM-chemistry
and looks very clean and bright.
It can't fail because of that.

I'm sorry for the bad English, hope you understand what I want to say.

 

[waltjr5858]

I know what you mean by the flowery smell but I can't tell you what it is. I have had that exact failure. Even using cucl2. The copper didn't cause your failure... it's something else.

 

[waltjr5858]

But I do know that no matter what amounts are used as long as you either scale down or scale up preferably from the original video that is up on this site there is a caption that comes up during the video that says you should add the p2np over the course of 6 hours. The only time this reaction has really worked good for me with very strong effects at the end except was still dirty and needed proper cleaning but it worked. Normal stuff water alcohol and borohydride all together and then I took whatever I was using at that time for the substrate p2np and divided it by 24. Whatever that equaled that's how much I added every 15 minutes until it was gone which was 6 hours. I noticed on the last addition that there was no reaction from the nabh4 fornsome reason? Guess I used it all up possibly so I added a half a gram of borohydride just in case. Waited 5 minutes and started dripping the proper amount of cucl2 in. When doing smaller reactions it's really hard to tell if you have added copper until the black particulate stops forming because the flask is small to begin with and the whole damn thing turns black. So as according to the video they used 25 or 26 G to 250 g of p2np so I did a 10 G reaction and it was somewhere around a gram or a little over of copper so I just dripped the entire thing in. Once I was done adding I just cranked the heat until I hit 80c and waited about 35 minutes and allowed it to cool to room temperature and it worked perfect minus being completely contaminated with some kind of Borate.. once I noticed that I just redesolved and acidified to a pH of 3 gave it a wash with nonpolar and then refreebased and gave it a little water wash. Dried it and re-added acid to crash out... it is a finicky reaction and definitely not as easy as most people put it there has to be some kind of trick as to the temperature you put your copper in the reaction or how long to let it react before adding the copper or something there's a trick to make it consistent because I can definitely tell you the aluminum Mercury reaction is very inconsistent even worse than this one