MDMA synthesis via NaBH4 from MDP2P

[chuckmcgill]

@G.Patton Hi thanks for your work! Do you have any advice on dissolving the MDMA freebase into DCM? Ours formed an apple sauce in the dcm (it tests purple black in marque reagant). We had dessicant in the mixture (mag sulfate) and used @btcboss2022 invitro methylamine HCL method but our organic layer is not homogenous so we are wondering if there are tricks thanks!

 

[2-79-790125]

saw you had an emulsion......looking for some tips:
Hi, I need help! : )

• Benzoquinone Wacker Oxidation of Safrole in Methanol to yield MDP2P
• From Erowid.org/archive/rhodium/chemistry/wacker.benzo-meoh.html
• By Methyl Man

Stuck on 5% NaOH Wash #2. Wash #1 was as expected, resulting in a very black top “aqueous?” layer that was discarded. When washing the bottom layer that presumably contains DCM and the Ketone with a 2nd 5% NaOH a massive amount of, I think, hydroquinone appeared. I drained the bottom layer to wash a third time, kept the top layer from 5%NaOH wash #2 just in case, and washed all the hydroquinone easily from the sep funnel. After adding the 3rd 5% NaOH Wash, I have a muddy green emulsion with zero separation.

Questions: Why didn’t the hydroquinone appear in the 1st wash?

Are my instructions 100% accurate that the top layer from the 1st 5%NaOH wash was “Aqueous” and therefore did NOT contain the Ketone and could be discarded? Or did I just throw away all my hard work and money?

Why does the emulsion seem to be getting worse with each NaOH wash instead of better?

What’s the best way to break up this emulsion?

Thanks. Its frustrating. Everything was going well up to this point.

 

[Win Win]

Can change methylamine hci to solution?

 

[G.Patton]

I don't understand your question.

 

[2-79-790125]

I had the same question. I have a stockpile of methylamine HCl . wondering how to use that correctly with this process.....

 

[malignoalfa]

I have DCM/Anhydrous Ethanol 60%/40% available. Can it be used?

 

[rothschild33]

Adding the NaBH4 manually over the course of a few hours is a bit cumbersome, I tried to dissolve NaBH4 in methanol then have this dripped into the RM with an addition funnel. The problem is that methanol reacts with NaBH4 pretty quick, decomposing. Is there another suitable solvent for NaBH4 or if I can add something to methanol to prevent decomposition while not affecting the reduction?

 

[inno]

Dear Mr., thank you very much for sharing the above methods. I also bought CAS: 28578-16-7, but my supplier only has powder and oily type, and there is no waxy form. I think I think Ask, can it be operated in the above method?
I expected that I will go to CAS 4676-39-5, and then to MDMA. The things that should be bought are already ready, but my NABH 4 has a swelling phenomenon in the packaging bag. Is it normal?

 

[everylittlehelps]

Sor
I don't understand this , how is gas weighted in grams or does is come in a powder form

--Methylamine gas (MeNH2) 300 g is dissolved in chilled 3000 g methanol (MeOH; -17-20 °C) in 20 L reactor, equipped with thermometer and overhead stirrer.

 

[G.Patton]

Hello. Gas can be weighted as other substances. You can multiply moles of the gas 22.4 to get its volume in dm3 (liters). https://en.wikipedia.org/wiki/Molar_volume

 

[inno]

Hello sir, thank you very much for sharing, I tried some small test pieces. Because I was in a hurry this time, I did not react it for two days, but for 4 hours. I used 50g of MDP2P oil to test, and finally only got 25g of MDMA base, and from this 25g of MDMA base, I finally got only 4g of white powder. .
I have encountered some questions and want to ask for advice:
1. Regarding the methylamine methanol solution, I used the wrong solution this time because I bought 33% pure solution. Can I use 33% solution in a 1:1 ratio instead of 10% solution?
2. Because I used 33% pure methylamine methanol, after I completed the NaBH4 reaction, when I used hydrochloric acid, the pH value could not be adjusted to 10.5~11. I used a lot of hydrochloric acid to adjust the pH value in place. It was normal. In this case, do I only need to use 8L of water and 8cc of 33% HCL for 1kgMDP2P to adjust the pH to 10.5 as described in your process?
3. In addition, when performing this step in the future, can I omit H2O and hydrochloric acid and use hydrochloric acid gas to make adjustments?
4. If the scale is expanded in the future, can I delete the final actions added by DCM? What will be affected? What are your thoughts on simple steps that can be taken to scale up?
5. Finally, what solvent can be used to dissolve the MDMA*HCL white powder precipitated from hydrochloric acid gas and perform recrystallization?

 

[G.Patton]

Hi. What do you mean 1:1? You need to take the same amount of methylamine free base. Are you able to calculate it? 1kg of 10% methylamine sln contain 100g of methylamine, 1kg of 30% methylamine sln contain 300 g of methylamine free base. How much 30% methylamine sln do you need to have 100g methylamine sln? School math.
Yes, I guess it's clear.

No, you need to use exact water volume.

You're gonna lose the yield.

It's already written in this topic. In addition, look at comment below.

 

[inno]

Dear Sir, thank you for your answer. I know that the specific gravity of 30% methylamine methanol solution required for each kg of MDP2P is 1100g, but the one I purchased from the supplier was 33%, so I converted it to 1:1. I hope there is no mistake. ,grateful.
My final question is, can I redissolve the MDMA*HCL powder in the photo in heated ethanol and saturate it so that it can aggregate into large crystals? Like meth?
Your answer is very helpful to me, thank you again.

 

[G.Patton]

No. You can't.

 

[YenaneY]

Is it possible to replace the acetone in the crystallization with something else? If yes which would be good alternatives?

 

[G.Patton]

Hi, yes. IPA.

 

[noMoneynoHoney234]

Can I use Methylamine aqueous solution 40% instead Methylamine (MeNH2) gas 300 g ？

 

[G.Patton]

Hello, you have to use methylamine methanol solution, water can't be added in this reaction. In opposite case, you won't get the product.

 

[noMoneynoHoney234]

can I replace this step with methylamine hydrochloride and methanol?

 

[G.Patton]

yes, you can buy ready made solution.

 

[lucas_cash]

Hey. Can you help me with something.

Is there a link on how to clean blackish mdma. Like recrystallize it and turn it more into white crystals? I think the freebase was not cleaned properly before crystallizing it.

The mdma is made from
Methylamine Gas
Methanol
Pmk
Sodium borohydride
Acetone and hcl

 

[G.Patton]

There is post about MDMA purification. Please, look at Amphetamine section.

P.S. It's really useful to look around or use Search instead of ask and wait an answer.