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

;-)

 

[Sciencenutz]

What was your yeild off this?

 

[btcboss2022]

From 966gr clean P2P I got 950gr of Meth oil
From 966gr of "dirty" P2P I got 800gr of Meth oil.

 

[Sciencenutz]

Isn't there 2mols of water produced for every 137g of p2p added? Plus the water from the methyalmine and lye produced and with 252g sodium sulfate I'm surprised this sucks all the water up I'll have to try this

 

[JuanoImano4378]

For this step, is it possible to add 30 teaspoonful of NaBH4 in minimum methanol in a big beaker, than drip it proportionately every 5 minutes instead of mixing a new batch every 5 minutes?

30 teaspoonful because 2.5hours / 5 mins is about 30 teaspoons, in case you're wondering.

 

[G.Patton]

yes, it is assumed

 

[Charlie3]

Can i use methylamine in ethanol instead of methylamine in methanol? my supplier sent me the wrong order.

 

[carbon_hydrogen]

Do i have to use Rotovap? because i dont have one or dont have money for it

 

[Zarder]

No, you do not need to use a rotovap

 

[boas]

How much could this be upscaled

 

[boas]

Whats the need for 2 10L Erlenmeyer

 

[G.Patton]

Hello, I don't understand your request, sorry. Please, reformulate your question clearly.

 

[bitcoinup2020]

In the synthesis process we either use a Reflux Condenser or mix it in a sealed round bottom flask.

Thank you very much for the answer.

I love BB

 

[UWe9o12jkied91d]

Do not ever seal a a reaction vessel, unless the procedure requires it, it is how you end up with an explosion.

 

[bitcoinup2020]

Thank you very much for the answer.

 

[Acab1312]

Is it possible to make the synthesis in a plastic Barrel?

 

[UWe9o12jkied91d]

Possibly, but if you want to work on a bigger scale in plastic you could work with stab? Much milder

 

[w2x3f5]

Are large metal barrels prohibited for sale in stores? =)

 

[Acab1312]

Ok I wrote to them, would be very interesting if it works ...

 

[masiuka]

Dear Colleagues.
I've read that some of you purify meth freebase by steam distillation.
I do not have enough efficient vacuum pump to keep water boiling poing below 60 deg.C so I thought I can instead wash it several times with distilled water.
To my surprise...first try of washing created emulsion that didn't want to break.
Eventually I added enough NaCl to create saturated solution and force the separation and I was able to recover freebase...
...anyway...
Can someone explain my how steam distillation can allow to get separated freebase and water layers and mixing it with water just gives my unbreakable emulsion?
I just don't get it. What's a difference??

 

[w2x3f5]

Use the solvent for extraction, dichloromethane, as an example.

 

[masiuka]

I see I did bad assumption thinking that steam distilled freebase will separate from water itself :-/
I combined the brine I had left with NaOH from reaction slury extract and I extracted it with IPA getting a little more of freebase.
The puny amount, I think, but, as Albert Hoffman said (starting his work in Sandoz), we need to learn working with small amount of chemicals ;-)

Thank you for quick advice

 

[w2x3f5]

alcohol draws water, better use dcm and use MgSO4 or Na2SO4 for dry solvent before distill