Methamphetamine synthesis from P2P by NaBH4 reduction. Medium-Scale.

[G.Patton]

No, you have to make free base only.

 

[Tweaker]

How did you prepare the methylamine freebase/methanol solution?

 

[G.Patton]

Hi. You can buy ready made solution or prepare it from methylamine hydrochloride by the following method: https://bbgate.com/posts/4279/

 

[Tweaker]

Thanks. I have HCl on hand.

 

[btcboss2022]

Hello,

After many tests using Methylamine HCL based on this method I will share the best way that I found to obtain Methamphetamine freebase in big scale:

• 966 gr P2P​
• 14 liters Methanol
• 1183 gr Methylamine HCL​
• 638gr NaOH​
• 452 gr Anhydrous Sodium Sulfate​
• 105 gr NaBH4​
• 35 L distilled water​
• 7 Liters DCM​

- Fill the reactor with the 14 L of Methanol
- With stirring dissolve the Methylamine HCL
- Put the reactor temp at 0C(not the mixture temp) and add the NaOH, the temp will increase
- Once the temp come back to 20C add the P2P, the temp will increase stir it during 45min-1 hour
- Add 252gr of anhydrous sodium sulfate
- When the mixture temp arrives to 8C start adding portionwise the NaBH4 not exceeding the 20C
- Once all the NaBH4 has been added let it mixing under 20C during aprox 2 hours until the mixture stops bubbling
- Add the water and continue mixing during 5 min
- Add the DCM and mix it during 10 min
- Stop stirring and let layers get separated
- Keep the bottom layer and discard the upper one( not profitable to extract this aqueous phase)
- Add 200gr of anhydrous sodium sulfate to the saved layer and mix it
- Filter it in Buchner Funnel
- Evaporate the DCM
- Clean and smelly Methamphetamine freebase obtained

;-)

 

[hunter12]

Do you filter the solution after adding anhydrous sodium sulfate?

 

[btcboss2022]

In my case no but you can do it without problems and take care with odor.

 

[hunter12]

Do you vacuum distill your oil freebase before crystallisation?

 

[btcboss2022]

No, I do steam distillation.

 

[Lordoftheshard 2]

So you can do an external steam distillation I asked this question I wanted to ad d dry caustic then steam distil the frebaae

 

[btcboss2022]

Yes you can do it anyway I'm not using NaBH4 route for Meth anymore.

 

[Acab1312]

Hello btcboss2022, what route are you going for meth now?

 

[Lordoftheshard 2]

Have you tried your cold method with Al/Ag yet

 

[btcboss2022]

Leuckart

 

[btcboss2022]

Not yet but I think it wont be a good method for big scale.

 

[wael gano]

where is she

 

[wael gano]

Your answer is incomprehensible

 

[btcboss2022]

No

 

[Tweaker]

I tried this method and didn't have the expected results. I have completed a very similar reaction with pmk with fantastic results. So I'm very confused.

mixture of methanol, methylamine and NaOH caused an evolution of gas and a milky white solution. Temperature rose and came back down.
P2P was added. Solution remained milky white with a brown swirl of p2p going through it as it mixed.
NaBh4 was added slowly temperature never rose over 10c. Mixture began to bubble and continued doing so for an hour until it ceased.

After extraction with DCM and evaporation a yellow oil was left with properties similar to the original P2p that was added.

 

[btcboss2022]

How much water added in the last step?
If you followed all in the same way and didn't works could be any of the reagents used no other option because a lot of people and myself did it hundreds of times.

 

[Tweaker]

Followed it exactly. I'm thinking maybe the methylamine escaped as a gas instead of being captured by the methanol

 

[BongMan]

can we smoke sulfate salt ..? i tried and sulfate salt is very easy to make just add H2SO4 10% and Acetone mixture and filter precipitate, wash with acetone to purify it...

 

[Ortist]

no sulphates can not be smoked. it will decompose before evaporation

 

[Tweaker]

Can you use mol sieves for drying?

 

[Ortist]

yes

 

[oneimone]

first part can be substituted by microwave radiation same like lpack with methylamine??