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

[Bartholomeus]

first picture after 6 hours leuckart reflux
second picture small amount of this 6 hours long reflux reaction poured inside separation funnel and cold water added to it

can anyone confirm this is good?
why is the n-formyl in separation yellow?
why is it not orange and clear?

should the reaction be run longer?
do you guys use the cooler in position like doing distillation, or just put the cooler on flask and run normal reflux?

@Hank Schrader @btcboss2022

 

[Hank Schrader]

You are not doing the first stage of the leuсkart correctly. Your color is not what it should be.
I think in fact you have a minimal amount of n-formylamphetamine in it.
The color should be a rich cognac color.
As I said earlier, the most important thing is to do the first stage correctly.
If you get 90%+ n-formylamphetamine, then the final hydrolysis will give you a huge yield.

 

[Bartholomeus]

Could you please tell me in short what to do in the first stage - turn the condenser to distillation way and distill of all the water slowly?
Then after all the water comes out turn the condenser to reflux setup and do the 6 hour reflux?
Or what am I doing wrong?
Cognac color should mean orange-brown?

 

[Hank Schrader]

color.

 

[blackburn]

Hi @ChingShih did you go further with hydrolysis?

 

[Bartholomeus]

No not yet

 

[Saul]

@ChingShih
you follow the formamide + formic acid 75% route ?
reflux is not important at the beginning off the reaction because off water .
boiling point from formamide is 220°c
Boiling point off formic acid 85% is 108°c
Boiling point off formic acid 75% is 100,7°c
for this reason it is allot better to use 85% pure formic acid
so if you start your reaction at 100°c the first hour or so
does your water evaporate first.

when the water is gone use the reflux and from then 6 hours cooking.

 

[OrgUnikum]

You might look up the boiling point of 75% formic acid. It is more like 117 °C as formic acid forms a high boiling azeotrope with water, not really intuitiv but thats how it is.

 

[Saul]

to people who also search for ansfers
there are different topics here on BB al starting from bmk salt to free base A-oil

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/need-help-convert-bmk-5449-12-7-to-free-base-a-oil.2906/

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/need-help-converting-5449-12-7-and-20320-59-6.1635/unread

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/p2p-synthesis-from-bmk-glycidate-ethers.4307/unread

 

[Saul]

@ChingShih react in private message to me. I share it with you ;-)
ChingShih say
I do the formamide + formic acid 85% route
But when the leuckart reaction heats up it is directly heated to 160 degrees celsius
it doesnt stay at 100 degrees like you wrote
so i dont know if the people first distill of water and then make the reflux or not
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ansfer

hello I know my friend but you need to take it at 100°c not higher the first hour
this is the only way to get rid off the water leftovers
becouse water boiling point is 100°c
and formic 85% boiling point is 108°c
after 1 hour use reflux

 

[TheNut22]

 

[KGB]

there is no need to distill anything if it heats up high enough,if reaction temperature drops too low and you cant heat it up then there is too much water in the reaction and only then you need to distill

 

[ossi]

hello,

"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."


I read here somewhere that hydrolysis with NaOH + methanol gives a much higher yield. can you confirm that?
if so, can you please describe in more detail?

thank you

 

[OrgUnikum]

For about 30 g Formylamphetamine:
150 ml Ethylalcohol (denaturated will do), 40g KOH and 35 ml water, reflux for 40 to 100 minutes, let cool down, acidify with diluted HCl, distill off Ethanol and a good amount of water (to remove steam-distillable impurities like P2P), let cool down a bit, basify with cold NaOH or KOH in water to ph >12, add enough water and steamdistill the Amphetamine out of the flask (steam-temperature as measured at condenser-entry is 94 to 98 °C - there must be always a lot of water in the flask to have this working well).
Thats much faster and told to be the best way to do the hydrolysis except for doing exactly the same in 5 to 15 minutes reflux in the microwave.
So I am told. I have insufficient experience with the Leuckart for a personal judgement though.

 

[blackburn]

A big thanks to @btcboss2022 for his help and this write-up. everything works as it should, the synthesis can be scaled linearly, with a very good result. and to all you haters who haven't even tried the synthesis/write-up, before you open your mouth and think you're experts, you can eat my shit!

 

[Davidrobinson]

What where the yields like you got my friend?

 

[blackburn]

Yield was around 70% without DCM extraction, after distillation. View attachment 13461

 

[blackburn]

 

[KGB]

what scale you did and what type of hydrolysis?the upper oil layer seems extremely thin

 

[blackburn]

Small scale, 100g p2p. Hydrolysis was NaOH.

 

[blackburn]

Also i want to note that i did not use Steam distillation, just regular distillation. At 120-130c

 

[OrgUnikum]

External overheated steam for sure considerably speeds the process up and I do not doubt that there will be more oil in the collection flask in the end. But I am afraid it is not more Amphetamine base but other stuff formed in the reaction. Amphetamine and Methamphetamine both distill with willingly with steam even from a just simmering flask and thats not just my imagination but it is well-documented in the literature.
This is more a point when somebody uses your base-hydrolysis method as when your acid-hydrolysis is used as in the acid hydrolysis you have a washing with DCM step before basification included which removes all non-basic unwanted stuff like leftover P2P, no such step is in the procedure with base.

Look, I want to express my gratitude for you posting this large scale method here, I seriously appreciate it very much and I want to assure you that what I write is intended to be constructive and no attempt to criticize you personally or to ridicule your abilities and achievements.

I do not know if you treat the oil from this reaction in any further ways, workup wise, for higher quality and to remove impurities or if you process it directly to "Paste" and however you do it, I am not here to judge, if your customers are happy they are happy.
For personal consumption I rather steamdistill very gently and then add some more steps but I am very old and got very sensitive to impurities in general.....

 

[btcboss2022]

Don't be afraid about this point I can assure you that there is more amphetamine base it's measured after solvent extraction.
In chemistry sometimes (not many) the literature differs a little from the synth reality and this is possibly one of those cases anyway I insist that you can check it yourself without problem and then comment it here.
About the solvent washing is an optional procedure since it will be steam distilled anyway and after distillation no impurities but even if you are afraid of impurities you always can make an acid-base washing when you extract the final freebase with solvent after distillation ;-)

 

[OrgUnikum]

Congratulations!

There seems to be quite some base in the water layer though, if you do not want to extract it you can add about the same amount of brine (saturated salt - NaCl - solution, easily prepared beforehand, this will press base out of the water layer and also suck some water from the base. Ideally the whole water layer would be saturated with salt but I suppose you are in a hurry so adding brine will do. You see the result after 5 to ten minutes, the water layer becoming clearer, but give it half an hour to do its job completely.