Complete amphetamine freebase (A-oil) synthesis from P2P(10L scale)

[blackburn]

Formic acid 85% work?

@btcboss2022

 

[41Dxflatline]

Formic acid 85% work?

@btcboss2022

SwesweYou use the formic acid on ammonium carbonate to produce ammonium formate which you can then use in the reaction to produce formamide in situ

 

[Davidrobinson]

Is that picture after internal steam distillation?
Did you distill your p2p for 70% yield , or did you use it straight from bmk ?

 

[blackburn]

Is that picture after internal steam distillation?
Did you distill your p2p for 70% yield , or did you use it straight from bmk ?

oscar412Yes it is .

I used The P2P immediately after conversion from 5449, i did not distill it.

 

[Tweaker]

Yes it is .

I used The P2P immediately after conversion from 5449, i did not distill it.

SwesweDo you have to adjust ph of p2p after conversion or you can use it as is?

 

[blackburn]

Do you have to adjust ph of p2p after conversion or you can use it as is?

TweakerYou can use it as it is...

 

[Tweaker]

You can use it as it is...

SwesweOkay I'm going to try again. First time I got a nice smelling yellow oil but after further processing got no finished product back. I think that my oil wasn't fully converted.

 

[blackburn]

Okay I'm going to try again. First time I got a nice smelling yellow oil but after further processing got no finished product back. I think that my oil wasn't fully converted.

TweakerOkey Good, what way you do , have pic?

 

[Tweaker]

Okey Good, what way you do , have pic?

SwesweI tried both hcl and phosphoric. Then nabh4 reduction both times. I'll dm you photos if I can find it

 

[tucoxXx1]

good afternoon ! I really like this synthesis, I've made it several times. but the yield when I need to get nform will be small at that point. I get 5L of nform from 10L of dirty P2P, and 1.5L from the aqueous layer. so in the end, after steam distillation, instead of 8.5 L yield, I always get 3-4 L. I do not clean the oil during any procedure. I think the steam will clean it. please anyone who can advise, thank you very much

 

[ossi]

good afternoon ! I really like this synthesis, I've made it several times. but the yield when I need to get nform will be small at that point. I get 5L of nform from 10L of dirty P2P, and 1.5L from the aqueous layer. so in the end, after steam distillation, instead of 8.5 L yield, I always get 3-4 L. I do not clean the oil during any procedure. I think the steam will clean it. please anyone who can advise, thank you very much

tucoxXx1N-Formylamphetamine Hydrolysis by NaOH way
1. Put the 11L of N-Formylamphetamine in the reactor, add 13L previous cold 65% NaOH solution slow stirring with reflux during 2-3 hours at 110C.
2. Stop heating and cool it at RT

use here methanol + less water and NaOH or KOH (for me KOH better), with methanol go to 85-90C.
you will see much difference

 

[ossi]

Could you explain please the proper ratios for methanol + lye solution + n-formyl derivate?
Why go only to 85-90C? And why to add methanol?
Do you mean it will be difference in yield or where will be the difference?
As I only tried normal Naoh hydro

Researcherrfor 1 liter n-formyl mix1,2-1,5 liter methanol, 700-850 gr KOH and 0,3-0,6 liter water. dissolve KOH complete. After it has cooled down a bit, put it in the fridge for a few hours. put this mix under stirring to the n-formyl and let mix half hour without heat. after go to 85-90C.
85-90 bacause boiling point from methanol is lower than water..
it will much more yield, i never would cook without methanol
and finally steam distillation is a must! (low temperature, more yield)
and you will get more yield , if you you use p2p formamid and little more formic acid.
if you have more formic acid you can cook at 140-145, this gives more yield.

 

[mr_pablitoescobar]

and what ph of that oil its is brother? and what weight per liter its being bro thanks

 

[Researcherr]

How much should be the weight of NaOH and Methanol ratio per 1L n-formyl?
If using NaOH instead of KOH?

@ossi

 

[btcboss2022]

How much should be the weight of NaOH and Methanol ratio per 1L n-formyl?
If using NaOH instead of KOH?

@ossi

Researcherr820gr NaOH Methanol 3 L

 

[Researcherr]

@btcboss2022 thanks for answer and how much water to add per this amount?
1L water - 820g NaOH - Methanol 3L - 1L n-formyl?
And why so much Methanol?

 

[btcboss2022]

@btcboss2022 thanks for answer and how much water to add per this amount?
1L water - 820g NaOH - Methanol 3L - 1L n-formyl?
And why so much Methanol?

Researcherr1:3 ratio with solvent is a very common ratio in different reactions, this is one of them.

 

[Researcherr]

1:3 ratio with solvent is a very common ratio in different reactions, this is one of them.

btcboss2022How much water to use for this ratio?

 

[Researcherr]

What about using:

Water 1L
Naoh 820g
Methanol 1L
N-formyl 1L

Would this ratio also be good?

 

[Researcherr]

Anyone with NaOH + Methanol hydrolisis experience please help with proper ratio of water, naoh, methanol, n-formyl

 

[btcboss2022]

Anyone with NaOH + Methanol hydrolisis experience please help with proper ratio of water, naoh, methanol, n-formyl

ResearcherrI told you but ok continue asking if needed no problem

 

[Researcherr]

@btcboss2022 yes i know you told me, but how much water to use per 820g naoh + 3l methanol? Or no water?

 

[TsssssXxX]

Hello. as far as I know, the cleaner the p2p and n-formamf are, the higher the yield will be in the end. I use p2p to clean; 2L of dirty p2p, I add 2L of hot water, mix vigorously, leave to choose a layer. upper layer is water, lower layer is p2p. is this enough? n-form cleaning: I slowly add a 10% baking soda solution to 2L of dirty n-form with strong mixing. I add it slowly because it foams strongly. I pour bicarbonate solution until I get a top layer. is this acceptable? thanks for the answers

 

[Sig]

Is this; 1. Put the 11L of N-Formylamphetamine in the reactor, add 13L previous cold 65% NaOH solution slow stirring with reflux during 2-3 hours at 110C. Possible in a glas reactor because today some one tell me it break the glas.(naoh solution) i only work before with steal reactor… its to expensive to try

 

[damakemi]

I added the 2 ways of N-Formylamphetamine Hydrolysis and as always is MY way and it works for ME don't means is the only and official way.

N-Formylamphetamine
​

1. Put 10L of P2P in the reactor, add 15L of formamide and 7L of formic acid, slow stirring with reflux during 5 hours at 140/150C.
2. Stop heating and cool it until a temp where you can add H2O without a big evaporation, add 13,33L of H2O mix and let separated the layers.
3. Keep the top layer(oil layer)
4. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 3, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
5. You should get around 11L of N-Formylamphetamine.

N-Formylamphetamine Hydrolysis by HCL way​

1. Put the 11L of N-Formylamphetamine in the reactor, add slowly 11L(1:1) of HCL 37%, slow stirring with reflux during 2 hours at 80/90C.
2. Stop heating and cool it until 25C, add 10L of DCM mix and let separated the layers.
3. Keep the top layer, bottom layer(DCM layer is discarded)
4. Add the cold top layer to a previous cold solution of 1,66kg of NaOH+ 2,66L of H20, let it cool at RT 12 hours.
5. 2 layers separated keep top layer(oil layer)
6. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 5, mix them and evaporate DCM.(Optional)
7. The mixture is steam distilled at 140-145C to get a transparent oil, at 100C oil starts to run out in the cooler at 130C turn on the steam and don't heat it more than 150C in that case you will get yellow oil.
8. Let separate completely the 2 layers of your distillation receiving flask, keep the top layer(oil layer)
9. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 8, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
10. 8,3L of amphetamine freebase obtained.

N-Formylamphetamine Hydrolysis by NaOH way
​

1. Put the 11L of N-Formylamphetamine in the reactor, add 13L previous cold 65% NaOH solution slow stirring with reflux during 2-3 hours at 110C.
2. Stop heating and cool it at RT
3. Keep the top layer(oil layer)
4. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 3, mix them and evaporate DCM.(Optional)
5. The mixture is steam distilled at 140-145C to get a transparent oil, at 100C oil starts to run out in the cooler at 130C turn on the steam and don't heat it more than 150C in that case you will get yellow oil.
6. Let separate completely the 2 layers of your distillation receiving flask, keep the top layer(oil layer)
7. Bottom layer( water layer) is extracted with DCM, let the layers separate completely, add the bottom layer(DCM layer) to the layer kept in the point 6, mix them, dry it with anhydrous Na2SO4 or MgSO4, filter it and evaporate DCM.(Optional)
8. 8,5L of amphetamine freebase obtained.

​

btcboss2022I did the Naoh way was wondering if it's possible to distill the oil right after 2-3 hours reflux, after point 2 ?

 

[btcboss2022]

I did the Naoh way was wondering if it's possible to distill the oil right after 2-3 hours reflux, after point 2 ?

damakemiSteam distillation yes.

 

[damakemi]

Steam distillation yes.

btcboss2022thanks for answering, can I make a larger amount of formamide and formic acid mix and store it?

 

[btcboss2022]

thanks for answering, can I make a larger amount of formamide and formic acid mix and store it?

damakemiwhat you mean exactly?