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

[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.

 

[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

 

[UWe9o12jkied91d]

n-formylamphetamine is a a slightly yellow oily liquid

 

[tweaker2]

you are propably right i was drunk throwing that stuff back of my head what i can remember and if i remeber correctly it was solid when cooled down

 

[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]

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

 

[tweaker2]

ammonium formate starts decomposing at 170-180c

 

[Davidrobinson]

Double check that, formamide is 180

 

[tweaker2]

yes formamide is but so is ammonium formate leuckart with formate is run between 135c-160c it varies some guys run it cooler some hotter

 

[Davidrobinson]

Ok. Whats the highest yields you have seen off the leuckart?

 

[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.

 

[Davidrobinson]

I promise u there is not i have ran hydrolsis at this ratio on this reaction. I can get you a number of write ups and articles what use this ratio also

 

[tweaker2]

the ratio is wayyy off maybe those write ups are done in micro scale did you calculate the molar ratio?if they really use that much acid it definetly is not concentrated and more likely diluted acid

 

[Davidrobinson]

Whats the highest yield you have seen off leuckart. I have only ever had 48% what about you. These yields are very high on this write up

 

[tweaker2]

yields were not very good anywhere from 700-800 grams dry amphetamine from 1 litre p2p if i remember correctly,we never calculated the oil we just salted it after distillation

 

[Davidrobinson]

I would say they are good yields

 

[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.

 

[Davidrobinson]

I would like to know tho btcboss, if you are using straight reflux or a dean and shark trap? Are you getting rid of the water ect ect?

 

[Saul]

hello @btcboss2022
what is the color off your N-formy ? pH ?

I found something very strange. my N-formy was dark brown
I keep my Ammonium carbonate ( mix ) from last time and there was just a little N-formy in the bottle on top layer
it was left over from separating maybe 5ml in a 1 liter bottle. Ammonium carbonate.
now 6 weeks later it is change from color to light orange and the amount is x3 minimum think 15ml

so maybe the ammonium carbonate way ( titrate ph7 ) is gold if you take your time
maybe we use to much heat and to little time .
anyway next time I start some weeks without heat then the heat and again let it stay a week and then separate

maybe monster yields

 

[btcboss2022]

I think you didn't read it my last post right?

 

[TheNut22]

Sometimes I heat my reaction mix about 4-5 hours, then I sleep. Again. Some sleep. etc etc ...
One time, the reaction took 5 days! There is some text in Festers Meth vol. 8:th, that if you leave the reaction mixture to stand for 4-5 days, and them heat it 160 C for 1 hour, it is complete! That was some Russian chemist IIRC ... Never tried that myself tho..

 

[damakemi]

You mean the p2p-formamide mixture was left for 4-5 days to form N-form? I would love somebody would test this

 

[TheNut22]

I haven't done that exactly. I have to be at work, so mostly I do my synthesis at night time...

 

[jokerr]

thanks, great master

 

[williwonkaa]

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.

​

Thank you. Could you tell me which reactor you took? Which materials do i need when i want to produce in big scale? 1000L reactor?
How do you heat the reactor?

 

[williwonkaa]

I