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

[blackburn]

Formic acid 85% work?

@btcboss2022

 

[41Dxflatline]

You 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]

Yes it is .

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

 

[Tweaker]

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

 

[blackburn]

You can use it as it is...

 

[Tweaker]

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.

 

[blackburn]

Okey Good, what way you do , have pic?

 

[Tweaker]

I 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]

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

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]

for 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.

 

[Researcherr]

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

@ossi

 

[btcboss2022]

820gr 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]

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

 

[Researcherr]

How 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]

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

 

[btcboss2022]

Steam distillation yes.

 

[damakemi]

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

 

[btcboss2022]

what you mean exactly?