Síntesis de anfetamina en una olla a partir de P2NP con NaBH4/CuCl2 (escala de 1 kg)

[SelfExper1menter]

Hola a todos. Intenté hacer un poco de anfetamina usando esta receta a pequeña escala, pero fracasé. Todo parecía estar bien, después del secado mi producto parecía polvo blanco con un tinte rojizo. Si se tratara de sulfato de anfetamina (que era lo que intentaba hacer), el rendimiento sería del 84%. El problema es que no es anfetamina.

Efectos fisiológicos
Probé 20-30 mg, definitivamente hubo estimulación, pero también causó fiebre y, aparentemente, una disminución de la inmunidad: las dos veces que lo tomé durante varios días seguidos, caí enfermo con infecciones respiratorias (la primera vez pensé que era una coincidencia). Otra persona que lo tomó no experimentó ningún estímulo con hasta 90 mg, sólo algo de sequedad en la boca. Ninguno de los dos tiene tolerancia a los estimulantes.

Pruebas químicas
1 g del polvo se disuelve completamente en 10 ml de H2O.
Cuando añadí un exceso de solución de NaOH a una masa medida del polvo en un tubo de ensayo, obtuve un volumen aproximadamente correcto de freebase con olor a amoníaco. Separé la capa de base libre, la sequé con CaCl2 e intenté valorarla con ácido. Como resultado, medí que la masa molar del freebase era de aproximadamente 171 (y para la anfetamina es de 135). Aunque mis mediciones no fueron muy precisas, la diferencia es demasiado grande para explicarla únicamente por errores de medición.

Mis desviaciones del procedimiento
1) Al añadir P2NP, me di cuenta de que iba a tardar horas, así que me impacienté y sumergí el matraz de reacción en un baño de agua a temperatura ambiente. Después pude añadir el P2NP casi de una vez, y la temperatura de la mezcla no superó los 40-50 °С.
2) Siguiendo el vídeo, no evaporé el IPA y añadí directamente ácido sulfúrico conc. a la capa de IPA/freebase.
3) No tenía acetona en ese momento, así que no la añadí antes de acidificar y lavé la pasta filtrada de "sulfato de anfetamina" con IPA.
4) El IPA es menos volátil que la acetona, así que tuve que meter mi precipitado en un horno durante varias horas para secarlo hasta peso constante. La temperatura en el horno no superó los 80 °С.

Entonces, la gran pregunta es, ¿dónde salió mal? No me sorprendería que el rendimiento fuera bajo o que no hubiera ningún producto, pero ¿obtener un buen rendimiento de una amina que no es anfetamina?

 

[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 no puede utilizarse con amina
1.en la primera etapa, el nitropropeno se reduce a nitropropano
2.impurezas recibidas de diversas sales en la composición de la pasta de anfetamina

 

[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