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

;-)

 

[Doubleboil]

and @G.Patton
Can I get some help please. I can’t get it to crystallise. Here’s what I’ve done more then a couple times.
methylamine hcl dissolved in Meoh
Naoh added and salt appears.
p2p added temp up and back down.
nabh4 on ice.
mgso4 normal
Water added and turns kinda foamy like milk
Dcm added
Separate take dcm layer. Color yellowish
MgSO4 and filter
Now this dcm layer has many small bubbles inside. (Air and product)?
Dcm is evaporated leaving a light golden oil.
Ph adjusted to 7 ( I’ve tried with ph 6 and 5 also)
Acetone added by
-3 to 1 ratio and freezer
-3 to 1 ratio air dry
-1 to 1 ratio and freezer
-1 to 1 ratio air dry


All of them failed. No crystals. Any insight would be appreciated. Thanks!

 

[mithyl2]

what can be used in place of Dichloromethane?

 

[Sciencenutz]

Toluene will be ok but it will be on the top layer then

 

[mithyl2]

do you think there would any adjustments to quantity I would need when using toluene?

 

[Sciencenutz]

Quantity as in volume needed to extract it all? I would just use same quantity as DCM and just keep extracting untill your toluene has no color therefore you extracted all the oil

 

[w2x3f5]

And if the synthesis is slightly changed, take water by desitylation of the alcohol / water azeotrope during the production of imine, and then use zeolite for better drying?

Why the color of coffee with milk? I always have a yellow color, I never got a brown color, not at the stage of imine formation, not at the stage of reduction with borohydride.

 

[Multivitamin]

hey i am newbie attempting this synthesis.I was wondering if my calculations are right.I want to scale it down to start only from 60grams of p2p oil.
These are my calculations:

p2p 60g
434ml methanol with 43g of MeNH2
15.6g magnesium sulfate
86,9 ml of silica gel
6,5g NaBH4
2 liters of water
434ml of DCM
0.2 l of acetone

Thank you for your time guys this forum is awesome.

 

[G.Patton]

Hello, correct. It isn't necessary to use exactly 15.6 MgSO4. You can use also Na2SO4.

 

[w2x3f5]

Better MgSO4, Na2SO4 not so fast work (

 

[mygodson]

An additional route, 3-phenyl-2-propanol and methansulfonyl chloride, and then react with methylamine can also yield the target product

 

[G.Patton]

Can you describe this method with details in detached new post? Or share a link please.

 

[mygodson]

An additional route, 3-phenyl-2-propanol and methansulfonyl chloride,
Triethylamine as alkali, in dichloromethane, raw material: methansulfonyl chloride: triethylamine mole ratio of 1:1.05:1.1, after treatment directly washing, steam can be directly to the next step.
Crude and tetrahydrofuran solution of methylamine reflux, the mole amount of methylamine should be at least twice, and then steam under reduced pressure, add dichloromethane or ethyl acetate, and then water, reduced pressure to remove the solvent can directly get the target product。

 

[Stretcher5335]

Mr mPatton or any expert please validate this claim. I dont know enough to say it is or it isnt but what i can say is it looks like the all to familiar cutting agent methylsulfonylmethane (MSM)

 

[G.Patton]

It is quite messy description. Nobody can repeat procedure by this manual =/

 

[mygodson]

 This is feasible.

 

[mygodson]

tell me your e-mail,I will tell you more about the operation process.

 

[G.Patton]

You can write me in DM here. If you want, you can encrypt this chat.

 

[mygodson]

how encrypt this chat

 

[mygodson]

 The by-product is methylamine mesylate，washed with water,then
can be removed

 

[w2x3f5]

The synthesis technique works, but constant problems with water, or silica gel takes part of the product.
The idea is to obtain an imine with simultaneous distillation of an azetropic mixture of IPA alcohol with water. Additionally, get rid of excess methylamine. An azeotropic mixture of IPA alcohol and water boils lower than absolute alcohol. And to dry imine add absolute alcohol, a small amount of silica gel, then borohydride.

 

[JuanoImano4378]

Hey G.Patton, what do you mean by "minimum methanol amount"? How do you determine the minimum here?

 

[G.Patton]

Hi, as minimum MeOH amount as possible to dissolve NaBH4 and wash out from drip funnel