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

 

[Davidrobinson]

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

 

[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]

Now I know what else I'm doing wrong, with synthesis with formate. Now I'm doing it with formamide, and right temperatures etc. Let's see how this goes when I'm done with the heating ...

 

[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.

 

[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

 

[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..

 

[MisterAnonymous]

@btcboss2022 your ratio calculation of hydrolysis with HCL is ABSURD!

Step 1: Calculate the Moles of N-Formylamphetamine

Assuming:
- **Density of N-formylamphetamine:** approximately 0.9 g/mL.
- **Molecular weight of N-formylamphetamine:** approximately 163 g/mol.

### Step 2: Calculate the Required Volume of 37% HCl

You need approximately 1 mole of HCl per mole of N-formylamphetamine for hydrolysis.

- **Concentration of 37% HCl:** ~12 M.

### Final Calculation:
You would need approximately **5.06 liters of 37% HCl** to hydrolyze 11 liters of N-formylamphetamine....