One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

[SelfExper1menter]

Hello everyone. I tried to make some amphetamine using this recipe on a small scale, but failed. Everything seemed ok, after drying my product looked like white powder with a tinge of redness. If it was amphetamine sulfate (which I was trying to make), the yield would be 84%. The problem is, it's not amphetamine.

Physiological effects
I tried 20-30 mg, there was definitely stimulation, but also it caused fever and, apparently, a decline in immunity: both times I took it for several days in a row, I fell ill with respiratory infections (first time I thought it was a coincidence). Another person that took it did not experience any stimulation from up to 90 mg, only some mouth dryness. Neither of us have any tolerance to stimulants.

Chemical testing
1 g of the powder completely dissolves in 10 ml H2O.
When I added excess NaOH solution to a measured mass of the powder in a test tube, I got an approximately right volume of freebase smelling of ammonia. I separated the freebase layer, dried it with CaCl2 and tried to titrate it with acid. As a result, I measured molar mass of the freebase to be about 171 (and for amphetamine it's 135). While my measurements weren't very precise, the difference is still too large to be explained by measurement errors alone.

My deviations from the procedure
1) When adding P2NP, I realized it was going to take hours, so I got impatient and immersed the reaction flask in a room temperature water bath. After that I was able to add P2NP almost all at once, and the temperature of the mixture didn't exceed 40-50 °С.
2) I was following the video, so I didn't evaporate the IPA and added conc. sulfuric acid to the IPA/freebase layer directly.
3) I didn't have any acetone at the moment, so I didn't add it before acidifying and I washed the filtered "amphetamine sulfate" paste with IPA.
4) IPA is less volatile than acetone, so I had to put my precipitate in an oven for several hours to dry it to constant weight. The temperature in the oven didn't exceed 80 °С.

So, the big question is, where did it go wrong? I wouldn't be surprised with low yield or no product at all, but getting a good yield of an amine that's not amphetamine?!

 

[poe]

Hello everyone. I tried to make some amphetamine using this recipe on a small scale, but failed. Everything seemed ok, after drying my product looked like white powder with a tinge of redness. If it was amphetamine sulfate (which I was trying to make), the yield would be 84%. The problem is, it's not amphetamine.

Physiological effects
I tried 20-30 mg, there was definitely stimulation, but also it caused fever and, apparently, a decline in immunity: both times I took it for several days in a row, I fell ill with respiratory infections (first time I thought it was a coincidence). Another person that took it did not experience any stimulation from up to 90 mg, only some mouth dryness. Neither of us have any tolerance to stimulants.

Chemical testing
1 g of the powder completely dissolves in 10 ml H2O.
When I added excess NaOH solution to a measured mass of the powder in a test tube, I got an approximately right volume of freebase smelling of ammonia. I separated the freebase layer, dried it with CaCl2 and tried to titrate it with acid. As a result, I measured molar mass of the freebase to be about 171 (and for amphetamine it's 135). While my measurements weren't very precise, the difference is still too large to be explained by measurement errors alone.

My deviations from the procedure
1) When adding P2NP, I realized it was going to take hours, so I got impatient and immersed the reaction flask in a room temperature water bath. After that I was able to add P2NP almost all at once, and the temperature of the mixture didn't exceed 40-50 °С.
2) I was following the video, so I didn't evaporate the IPA and added conc. sulfuric acid to the IPA/freebase layer directly.
3) I didn't have any acetone at the moment, so I didn't add it before acidifying and I washed the filtered "amphetamine sulfate" paste with IPA.
4) IPA is less volatile than acetone, so I had to put my precipitate in an oven for several hours to dry it to constant weight. The temperature in the oven didn't exceed 80 °С.

So, the big question is, where did it go wrong? I wouldn't be surprised with low yield or no product at all, but getting a good yield of an amine that's not amphetamine?!

SelfExper1menterDid you get your answer? I am interested in knowing what went wrong also.

 

[tucoXxX]

Hello. add nabh4, I turn on the mixer. What is the recommended mixing speed (rpm)? can the speed be the same while administering nabh4, p2np, cucl2? Step 5: keep warm for 30 minutes at 80 degrees, is mixing necessary here? Thank you for your answers

 

[UWe9o12jkied91d]

Hello. add nabh4, I turn on the mixer. What is the recommended mixing speed (rpm)? can the speed be the same while administering nabh4, p2np, cucl2? Step 5: keep warm for 30 minutes at 80 degrees, is mixing necessary here? Thank you for your answers

tucoXxXStirring should be applied troughout, the more stirring the more H evolution, so decrease as necessary

 

[poe]

Can you also use the sludge to produce amphetamine? If so, what steps would you take? Dry acetone and sulfuric acid?

 

[poe]

what are alternative supplies for this synthesis? Something someone can obtain from a hardware store.

 

[Marvin "Popcorn" Sutton]

what are alternative supplies for this synthesis? Something someone can obtain from a hardware store.

poeOf course you can buy some reagents in a hardware store, but you will never buy P2NP there.

 

[tucoXxX]

this would be the aqueous layer. I added 25% naoh solution. which layer do i need ?? I was a little confused

 

[Marvin "Popcorn" Sutton]

this would be the aqueous layer. I added 25% naoh solution. which layer do i need ?? I was a little confused

tucoXxXWrite down what proportions of reagents you used.
How long does the mixture stand after adding the NaOH solution in the photo?

 

[tucoXxX]

Write down what proportions of reagents you used.
How long does the mixture stand after adding the NaOH solution in the photo?

Marvin "Popcorn" SuttonHello. 10L IPA
Distilled water 3.1 L;
Sodium borohydride (NaBH4) 870 g;
P2NP (Phenyl-2-propanone) 500 g;
Copper (II) chloride (CuCl2) 52 g.
Sodium hydroxide (NaOH) water solution 25% 4 L;. these reagents . this was the bottom layer (water layer). I added Ipa these layers are formed. I let it rest for 10 minutes

 

[w2x3f5]

Hello. 10L IPA
Distilled water 3.1 L;
Sodium borohydride (NaBH4) 870 g;
P2NP (Phenyl-2-propanone) 500 g;
Copper (II) chloride (CuCl2) 52 g.
Sodium hydroxide (NaOH) water solution 25% 4 L;. these reagents . this was the bottom layer (water layer). I added Ipa these layers are formed. I let it rest for 10 minutes

tucoXxXif the alkaline amine goes into the upper alcohol layer. if ph is acidic, it will be in the lower layer in the form of a dissolved salt. In any case, there will be losses with this method of allocation.

 

[tucoXxX]

Write down what proportions of reagents you used.
How long does the mixture stand after adding the NaOH solution in the photo?

Marvin "Popcorn" Suttonabout 2 minutes and two layers are formed, I leave it alone for 30 minutes.

1754g nabh4
1000g p2np
100g cucl2

 

[mithyl2]

is it necessary to stir for 6 hours while you add the P2NP, or do you only stir for as long as it takes to dissolve it safely?

 

[ACAB]

is it necessary to stir for 6 hours while you add the P2NP, or do you only stir for as long as it takes to dissolve it safely?

mithyl2For best results use overhead steering for flask.

 

[mithyl2]

For best results use overhead steering for flask.

ACABok, but is it necessary to stir for 6 hours while you add the P2NP, or do you only stir for as long as it takes to dissolve it safely?

 

[mithyl2]

For best results use overhead steering for flask.

ACABand i was hoping to be able to use the magnetic stirrer lol. but i had my doubts about whether it would be strong enough.

 

[ACAB]

and i was hoping to be able to use the magnetic stirrer lol. but i had my doubts about whether it would be strong enough.

mithyl2It could take 6 hour, take time for synthesis, take attention with temperature.

It depends on how much aluminum is in the flask and how good your magnetic stirrer is.
Overhead stirrers have more power.

 

[Marvin "Popcorn" Sutton]

Use intermittent stirring during synthesis if you cannot stir continuously.
After adding NaOH, stir the mixture well and leave it alone to allow the layers to separate.

 

[tucoXxX]

Hello. 10L IPA
Distilled water 3.1 L;
Sodium borohydride (NaBH4) 870 g;
P2NP (Phenyl-2-propanone) 500 g;
Copper (II) chloride (CuCl2) 52 g.
Sodium hydroxide (NaOH) water solution 25% 4 L; I use these reagents. I observe temperature regulation. I add it to 4L of 25% naoh reaction mixture. how much should the reaction mixture be cooled when I add naoh? top layer (orange) is a mixture of Ipa / base. bottom layer (black) water layer right? Rotovap is poured into the IPA/base mixture (vacuum, cooling equipment in one equipment). I pour in 3 liters of Ipa / base mixture, how long should it be evaporated? how much should the flask remain? I don't want to evaporate the base, how many degrees should I not exceed? then I take the aqueous layer and add 4L IPA. I mix and let the layers separate. which layer will I need? top orange bottom layer or clear cloudy ? I put a suitable layer in rotovap and remove Ipa. after that I combine two layers. Unfortunately, I do not have a degree in chemistry, this is where I found the courage to prepare this synthesis. Please, if you answer, describe that you are talking to a beginner member, that way I understand. thanks for the help !!!!

 

[csigger]

If I feel that not all p2np is converted, can I increase the amount of nabh4? What happens if I only give more of that, everything else remains as described.

 

[tucoXxX]

I want to make bmk oil, could you help me?

 

[tucoXxX]

hello gentlemen !

The IPA from step 7 extract is evaporated on vacuum to an amphetamine free base oil and combined with free base from step 6.

I evaporated it into my vacuum and this is what I got. this is good ? (first picture) what to do with this, because it doesn't smell like an amf. should I add it to the free base?

And Ipa/free base is evaporated to get better quality oil. (image 2). my first synthesis, I hope I was successful ....

should I mix the two at the end??? hmm, I don't understand.

 

[tucoXxX]

Ipa párolgás után így néz ki az Ipa/free base. majdnem 6 liter volt. amikor elkezdtem világosabb volt a színe és kellemes illata volt, erősebb mint most. lehet, hogy elégettem az alapot??

 

[tucoXxX]

This is what Ipa/free base looks like after Ipa evaporation. it was almost 6 liters. when I started, the color was lighter and it had a pleasant smell, stronger than now. maybe i burned the base??

 

[tucoXxX]

I don't think you should do anything with the IPA/base after the election. there is too much alcohol in it, I would like to reduce the ipa. I think the quality of the oil may be poor due to too much IPA.

 

[WinterDust]

I don't think you should do anything with the IPA/base after the election. there is too much alcohol in it, I would like to reduce the ipa. I think the quality of the oil may be poor due to too much IPA.

tucoXxXYou are wrong.