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

[btcboss2022]

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.

​

 

[btcboss2022]

I forgot to add that you must be careful with ammonia odor and fumes in the NaOH way ;-)

 

[Davidrobinson]

That is a good yield, how long is it taking you to steam distill 8.5L of freebase?

 

[btcboss2022]

Many hours but depends on equipment too, in my case I need to wait 1 hour only to have the steam at the temperature needed, thats is the worst part of the process honestly but everybody have the same "problem" when you need to distill oil with water even steaming.

 

[sankharaKokosDreams]

so you did not do it ?
it is a simple question.

 

[btcboss2022]

Ok ok you caught me I didn't do it is impossible to deceive people as intelligent as you sankharaKokosDreams, tweaker2... do not know how you haven't discovered me before!
Thank you to share your valuable time in the forum because your detective skills they are up to the task of the FBI, DEA,EUROPOL...

Now that you uncovered me I will explain you the truth:

I'm just a boring teenager without work, without friends and afraid to go outside. The only contact with the world is my computer.
I had to leave high school because they messed with me,laughed at me...

I saw Breaking Bad in Netflix and later I found this forum and I thought it might be fun to post fake information, synthesis, pics...and imagine people face after doing a totally invented synthesis. You don't know what I've come to laugh imagining these faces hahahaah how stupids are they

Now that you have hunted me I don't know what I will do during all day this forum was my main entertainment, I don't know if I can overcome it and I'm afraid of doing something crazy against myself. If that happens it will fall on your consciences and you should live with it.

PD: For those who do not understand this message, I summarize it:

I won't post anything else, or help anyone by PM or any other way that is what you achieved by treating like this altruistic people without any type of economic or personal interest just the encouragement to share experiences. Could be a possible situation to be considered by Forum admins to try to avoid futures ones if they consider it appropriate. Anyway you will live without me don't worry all will be ok.
Good luck and thanks.

 

[UWe9o12jkied91d]

reactor size? 50L ?

 

[btcboss2022]

I use 100l but with larger amounts 50l more than enough for the synth posted.

 

[ossi]

hello,

thanks for your effort.
H2O mix with what? i don't understand this

 

[Davidrobinson]

Add h20 to the reaction. Read it, how dont you understand that. Its a very good write up.
And the best yield i have see reported for the Leuckart

 

[ossi]

now understand, he mean mix this. i understood before h20 mix. because comma

 

[blackburn]

Formic acid 85% work?

@btcboss2022

 

[blackburn]

Is it also possible to replace fomamide with something else

/Thanks

 

[UWe9o12jkied91d]

formamide is the key to these yields

 

[btcboss2022]

Is possible with carbonate ammonia but the process is different having previous steps.

 

[btcboss2022]

I doubt you can find formic higher than 85% ;-)

 

[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

 

[Bartholomeus]

@btcboss2022 when you say turn on the steam at 130C this means that the mixture which we distill is at this temperature and then we add the steam to it from another source(which is normal steam with temperature 100C right)?

 

[btcboss2022]

Steam could be at different temperatures depending on pressure outflow, more pressure more temp.
I use a heating source not only the steam, if you have the enough pressure and temp in the Steam possibly would work without the heating source but I never test It.
I think is easier to find a heating source than an equipment with the necessary pressure and temp for the steam at least at large scale.

 

[tweaker2]

this writeup is trash.first of all the temperature with formamide is too low 140-150 sounds about right if u are using ammonium formate but formamide needs higher temp if i remember correctly and secondly N-Formylamphetamine is solid mass not liquid and why would you try to extract it from the reaction mixture completely useless step it only hurts your yields third your hydrolysis is wrong you are using 11l hcl that is insane even if you had 11 kilos of N-Formylamphetamine the amount would be close 2,5 liters of hcl not 11l its 1:1 by molar mass not by volume.why do you make everything so complicating Leuckart is simple reflux hydrolysis and then basify and then steam distill all in same pot so no extractions or solvents are are needed i highly doubt that you have ever done this reaction and if you have your yields are close to zero if you do it as you say.okay merry xmas to all im going to sleep im drunk as hell

 

[btcboss2022]

First sentence of my post:
"MY way and it works for ME don't means is the only and official way"
Anyway if you have Big doubts about if I did It or not you are invited to check It Im always open to learn ;-) we could find the way that you come to my place.
And honestly in all the synth tested I never had a solid N-formylamphetamine could be interesting. Thanks.

 

[Davidrobinson]

If you ran a leuckart at 140 150 with ammoina formate it would only break down into formamide anyway

 

[TheNut22]

I totally agree. Some russian chemists do the Leuckart with ammonium formate even as low temp
as 120 C. I do mine 140-150 C with ammonium formate. With formamide, the temp is around 155-165 C. Even if formate brakes to formamide, there is different temp and mechanism with those two reagents.

 

[TheNut22]

It is different synthesis with formate, if you don't want it to convert to formamide "in-situ".

 

[UWe9o12jkied91d]

n-formylamphetamine is a a slightly yellow oily liquid

 

[TheNut22]

It went to trash. I don't know what the hell is wrong with my Leuckart.. Reaction time 20 hours, temp: 150-160 C (formamide), and all reagents were in right amounts. Is it that my magnetic stirrer is broke and I don't stirr it more often, or what. My N-Formyl amine is always black. Do I burn it? And when I do base hydrolysis, there is not much if any ammonia gas produced, so my N-formyl "amine" is not at amine at all?! Can someone help me. My P2P was 8 grams amount + other reagents.

 

[TheNut22]

OK. What was wrong, it was my so called "P2P", witch was not P2P.

 

[Davidrobinson]

And theres nothing wrong with the amount of acid for hydrolsis . Have you done this synthesis before tweaker?

 

[tweaker2]

nothing wrong with hydrolysis?Yes there is almost everything.yes i have done this synthesis with my friend long time ago.

 

[TheNut22]

What OrgUnikum will say about this, I don't care, but I have papers, that shows that ZnCl2 and AlCl3 are good catalysts in Leuckart reaction.

 

[OrgUnikum]

I say that I honestly wish it works. I have read articles and patents about the Leuckart en masse with or without catalyst, with or without Voodoo ceremonies but I have not seen it working. Claimed 95% yields with Nickel as catalyst which were once posted came out to be just not true, sadly.
I dismissed AlCl3 first as it is if anhydrous so very hygroscopic and not much a catalyst when wet, but on a second thought this holding on to water might be the key that it works and not any catalytic function. As the reaction needs water but also temperatures where all water gets expelled what is contradicting. AlCl3 holds on to water so strongly that even at the high temperatures needed there will be still water bound bei AlCl3 and this is still available for the reaction to proceed. An interesting twist.