PMK Oil Synthesys From PMK (CAS 28578-16-7 Wax Form) Large Scale

[btcboss2022]

Hello,

After check and test the methods posted in the thread http://bbzzzsvqcrqtki6umym6itiixfhn...-methyl-pmk-glycidate-conversion-to-pmk.2013/ I decided the post the best method for me:

1. Put 47,5 liters of H2O in the reactor and add 2,5kg of sodium bicarbonate, stirring until complete dissolution, take out the mixture and keep it.
2. Put in the reactor 7L of H2O
3. Add while stirring 1,2kg of sodium hydroxide
4. While the H2O and the sodium hydroxide are mixing and getting temp put 5kG of wax PMK to melt by low heat.
5. When PMK is melted add it to the reactor and put the mixture at 80 °C reflux during 1 hour stirring.
6. Add 3,25kg of HCL 37% in small portions, once all added keep the mixture at 80 °C reflux during 1 hour stirring.
7. Stop stirring and put the mixture at 25 °C.
8. Discard the water top layer.
9. Put again in the reactor the oil top layer.
10. Add the H2O and sodium bicarbonate mixture, stirring 2-3 minutes.
11. Add 10 liters of DCM (from freezer preferably).
12. Let it get separated around 10-15 min.
13. Evaporate DCM from the bottom layer.

PMK oil (MDP2P; cas 4676-39-5) yield is 3,72kg.

 

[G.Patton]

Reaction scheme:

 

[Bartholomeus]

You always Impress with those complete synthesis reports, keep it up brother! Congratulation on success

 

[Bennychairman]

Thanks for saving us time ! just got mine , so just in time. thanks a lot !

 

[Bennychairman]

8. Discard the water top layer.
9. Put again in the reactor the oil top layer.

how many layers will there be? the top was discarded water and then ?

 

[Field7]

I saw that, too. That's a typo. There should just be two layers. I'd expect the oil layer to fall to the bottom. Separate the top, aquas layer, and discard. Keep the bottom oil layer for the next step. Then, later, if using DCM, your end product will be in the non-aquas bottom DCM layer. If you substitute Toluene or Diethyl Ether for DCM (like someone else asked about doing), your product will be in the non-aquas upper layer. DCM, down. Toluene and Diethyl Ether, up. I'd suggest you stick with DCM because it can be separated using low heat unlike Toluene, and doesn't pose quite the same fire hazard that DE does. It is a carcinogen, though, and *does have a low flash point*. Use a well ventilated space, and collect in a chilled vessel for reuse.

 

[btcboss2022]

2 layers, when you discard water layer you must wash the oil layer with water+sodium bicarbonate solution as the procedure explains.

 

[Dafunkphenomena]

Hello , thats my method, (im Fring, just lost the fucking password)
ive seen you added some steps, questions:

you deceided to use sodium bicarbonate instead of NaOH washings , why exactly? (i tried both all worked)
and in the final step, you say "evaporate the DCM from the bottom" , why evaporate? would not be better separate the layers?
or you mean , after separate put it to vacuum distill to get rid of some possible water residues?

and the PMK colour? dark red-brown, or yellowish as the old one?

 

[Field7]

You do separate it. You separate the bottom layer, which is composed of DCM and Product, and then evaporate the DCM from *what was the bottom layer* (I'd use a hot water bath) to leave your (dirty, but clean enough for most) product. Steam distillion of the product would be a good idea, I think.

If someone is familiar with the chemistry, they know there's a bundle of variations you could apply.

 

[Curiousonion]

Does this method work, did anyone try this?
Seems by far the simplest method and too easy.

 

[Curiousonion]

Well this method is for pmk CAS 28578-16. So you can get that in powder form then it turns into oil after you finish with the reaction.
But this seems extremely easy, has anyone tried this?

 

[Bartholomeus]

The method is proven and this is why the OP posted it, try for yourself and see

 

[Curiousonion]

Perfect, I shall. Just wanted to make sure because there seems to be a lot of confusion about pmk oil and its different versions.
Thanks

 

[G.Patton]

This post is good explanation, which was posted @btcboss2022 (thank you). I confirm, that it is proved and working method.

 

[FredDurst]

Is there any alternative to DCM (Toluene maybe?) as its hard to get in my country?

 

[Precursor-supplier]

I can provide

 

[Jordan Belfort]

boiling of tolueen is problem.

 

[Curiousonion]

That's fantastic, maybe this needs to be made a sticky since it's so useful?

 

[btcboss2022]

Hello,

Sorry I was very busy these days, all the methods that I posted have been done and tested by myself as I say in the same post, it's more many of them tested and only the best one posted.
Thanks.

 

[Handsomerx]

Why is there no reference to color of the oil and aqueous phases?

 

[btcboss2022]

Im not used to reference them but what do you need to know exactly?

 

[Handsomerx]

Like what is the color of the oil which separates to the bottom? My starting pmk is kind of a light brown color so I assume the oil which renders out should look similar to that.
What is the color of the aqueous layer upon separation? Mine is a sort of pale yellow green.

I thought it was standard operating procedure to mention the color of your product.
Anyway thank you! It’d be very helpful to hear back.

Side note…when you say “evaporate dcm” do you mean actually to let it sit with low heat to evaporate? Or are you talking about stripping it under vacuum.

thanks

 

[btcboss2022]

Hello,

Firstly I don't think you created that process, in fact I had this similar info long time ago from Chinese suppliers, anyway I made some changes as you can see.
Sodium bicarbonate is a softer washing method and in this case is safer to use it to avoid to damage the product.
About DCM obviously I mean to separate the bottom layer(DCM layer) and evaporate it sorry if my explanation is not clear.
To avoid water after separate layers you can dry it with anydrous sodium sulfate and filter it before evaporate the solvent( in fact I always do it in all my processes)
Thanks.

 

[FredDurst]

Is there any alternative to DCM (Toluene maybe?) as its hard to get in my country?

 

[btcboss2022]

Toluene will works too but I can't assure you the same yield basically because I didn't tried.

 

[FredDurst]

Ok thanks mate. Will give it a go

 

[Curiousonion]

May I ask what method you use to crysyalize the final product?

 

[btcboss2022]

Before crystalize you must get the freebase, for freebase I use NaBH4 method and to crystalize the freebase there are a lot of methods.

 

[MisterAnonymous]

Is this synthesis for in 50 or a 100L Reactor?
@btcboss2022

 

[Curiousonion]

Ah ok so I was confused, I thought the final product that you got from your reaction was the mdma freebase.

 

[Curiousonion]

Do you use ammonium acetate for the reduction or MeNH2 gas?

 

[Field7]

+ Ammonium Acetate = MDA
+ MeNH2 = MDMA

Up to you.

 

[Dafunkphenomena]

i assume you are not following the hcl gas route , but im curious, why you cristallize the free-base?