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

[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

;-)

 

[chef learner]

I would like to ask about the methylamine HCL in the list. Should I add methylamine HCL directly or convert it into methylamine free base (methanol solution) and then add it?

 

[chef learner]

In this method of BOSS, apart from the water problem, is there anything else that will affect the yield?
Why is the yield of methyl free base remaining after evaporating DCM only 50%?
Is there anything I should pay attention to that I haven’t noticed? Please help me~~

@G.Patton

 

[chef learner]

Is the MDP2P produced by this method suitable for making methamphetamine?

If applicable, is the extracted methamphetamine free base directly acidified and crystallized?

 

[btcboss2022]

Not exactly, you will obtain D-meth freebase.

 

[chef learner]

What kind of crystals crystallize after stirring with L-tartaric acid?
Levomethamphetamine?

Can the remaining liquid d-methyl free base (PH12~13) after vacuum filtration recrystallize into D-methylamphetamine after acidification? If so, what approach should I take?

 

[btcboss2022]

What kind of crystals crystallize after stirring with L-tartaric acid?
Levomethamphetamine?
Yes and tartaric ones.

Can the remaining liquid d-methyl free base (PH12~13) after vacuum filtration recrystallize into D-methylamphetamine after acidification? If so, what approach should I take?
Read the process please is detailed and is not in this way.

 

[chef learner]

Hello, BOSS, I carefully read through each post and the reply area. I want to know whether my project plan is correct and feasible.
Make BMK oil -> Use your method to make methamphetamine free base -> Tartaric acid separation -> Obtain (L or D) methyl free base -> Add NaOH to raise the pH (12~13) -> (What are the steps required at this time Acidification to obtain crystals), maybe I didn't notice it, but I'm not sure which method is most suitable for acidification and crystallization at this time. Can I ask you for an answer?
Thank you

 

[rifta]

Hello .
For the methylamine solution i have mixed methylamine hydrochloride+ naoh + mgso4 in methanol ,i see a little réaction of heat, but now 24h after i have a lot of solid on the bottom, maybe unreacted methylamine hydrochloride and naoh
Dis you think i need to add the mgso4 after the methylamine hydrochloride naoh réaction ?
Thanks

 

[btcboss2022]

Yes you need it to dry the water generated in the reaction. You can filter the solid.

 

[rifta]

Yes i know ,the réaction is water sensitive, my problem is i have added the mgso4 at the same time with the methylamine and the naoh not like your protocol, you added it after the methylamine hcl naoh réaction,did you think i make an error ,i have a lot of powder at the bottom maybe unreacted methylamine hcl , thanks for your response

 

[chef learner]

I think what you are talking about is the NaCL produced when making methylamine free base, which needs to be filtered out.

 

[ImRegistered]

Has anyone scaled this up?
what would the measurements be for methanol/methylamine in a 5000g p2p synthesis?
The current 36 liters ratio sounds over kill

 

[G.Patton]

Hi, upscale proportionately. I don't recommend to do large batch if you haven't tried small scale.