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

[btcboss2022]

Hello,

Here is my last achievement make it to crystallize naturally in the molecular form of the crystal itself. More pure impossible!! ;-)
Seems handmade but trust me are naturally formed!

 

[Tweaker]

Very nice work. What process do you use to remove the black tar like impurity? Even on snow white crystals it appears on subsequent recrystalizations and the end product becomes quite dark.

 

[Tweaker]

You do a second acid base to remove the black substance? When I gas the freebase crystals are snow white but turn dark and contain that sticky substance after recrystalization to large shards. The dirty acetone used to wash also contains a lot of this and mdma. I've thought of trying to distill the freebase before crystalizing.

 

[Jordan Belfort]

Your p was yellow and not white correct?

 

[Tweaker]

Wax was the brown one. Old stock. New yellow one is much cleaner I hear. Haven't had the chance to run this yet.

 

[btcboss2022]

I only do it once possibly precursor quality affects this I always use powder wax is more dirty I had it at the beggining too.
Yes your best option is steam distillation.
I checked and seems that impurity is mdp2ppol or similar but name is not important in that case.

 

[Tweaker]

Okay thanks sounds like powder is the way to go. I have a sample amount of powder the conversion method is identical to wax?

 

[btcboss2022]

Yes exactly the same.

 

[axecap168]

Btcboss2022, please help I followed your recipe for synthesis of pmk 28578-16-7 powder to mdp2p and after refluxing oil separation occur but there was still some white cloudy stuff in the oil and as the oil cooled the white cloudy stuff became thicker like soggy cereal and left me with very little oil.
Has anyone seen this happen before?
What did I do wrong btcboss2022?
Can anyone help me with this?
I have attached some photos.

 

[Jordan Belfort]

Redo reaction with little more water assume you did with hcl ?

 

[btcboss2022]

OMG! Should be destiny or something similar hahhaah
I never had any issues in more than one year with that process and last week happened me the same with a 15kg powder batch(was the last 15kg of a large batch so same product)
I'm at 99% sure that is about storage and storage time, in my case I stored in a bucket with lid around 6 months.
I isolated that solid that seems a kind of polymerization of the original stuff.

I tested with what product it gets solved:
Water: No
Acid water: No
Alkali water: Practically nothing
DCM: No
Methanol: Practically nothing
Acetone: No

Strange right? It only gets liquid at high temp or with hot water similar to the original stuff so the only 2 options are:
- Unreacted product ( very improbable after hundreds of times of performing the same process also with the same batch, and it must be solved in alkali water too)
- A kind of polymerization due the storage time and conditions.

You can try more time at 90C with the HCL but I guess it wont works.

What I did( don't means that is the solution or that you must do the same)

I added water stir it and later DCM and all in a separator funnel.
You will have the top layer water, middle layer the solid and bottom layer the DCM+PMK oil later later evaporate DCM.
It is a slow separation and I did it 3 times with DCM.
Obviously the yield is much lower than normally but better this than nothing.

I'm sorry couldn't help you more I had the same problem and I tried to fix it as best I know using the common sense and my previous experiences.

Possibly a chemist would help you in a better way.

 

[axecap168]

Belfort, thats correct reaction with HCL.

 

[axecap168]

Btcboss2022
Thank you for the reply to my post. The powder came in wrapped thick plastic bag in a cardboard box as usual. I only received it 1.5months ago but how long in storage before me, who knows. I store it in a cool room temp space. I did 2 reactions in total, 1 reaction from 1 box and anothe reaction from another box with the same results. I guess this batch is compromised. I agree with "something is better then nothing"
You said "I added water stir it and later DCM and all in a separator funnel."
Question...
1. What was the ratio of water and dcm you added to the oil and how long you stirred it?
2. How much less was the yield?
I will try 90C or higher temp with HCL at longer duration as you suggested. If I find solution I will post it here and let you know.

 

[axecap168]

G.Patton, Gordon Ramsey or any chemist in this community - can you offer any solutions to this problem? Any help is greatly appreciated. Thanks in advance.

 

[Jordan Belfort]

Get white phosphorus acid and stirrir ontop in stainless steel pan and just put all together and heat at 80/90 you see reaction going and then after few hours reacting wash the phosphorus acid off till pH 7.

 

[axecap168]

Belfort, thanks. I will try your suggestion out.

 

[blackburn]

@btcboss2022 Will there be a writeup from your way of MDMA Synthesis from PMK oil (MDP2P: cas 4676-39-5)


/ Thanks

 

[btcboss2022]

I writeup about if the precursor is not in good conditions you could have a solid in the process?
In that case all processes should have it right?

 

[Paranoia]

Coming next @btcboss2022 lab test for ICE PURITY & ENIANTOMETER R,S come back to be updated

Energy Control

analisis2.energycontrol.org

 

[CryoThio]

Can one replace the bicarbonate solution with a lesser amount of a hydroxide solution, assuming they are the same ph?

 

[Jordan Belfort]

Baking soda neutralize the acid, but to much baking soda makes the remaining baking soda in the oil, which you only can get out by distillation or puting acid again and lye the last part

 

[CryoThio]

So if the purpose is to neutralize the acid, why wouldn't a sodium hydroxide solution be able to replace the bicarbonate solution, assuming they are the same ph?

I just don't understand why such a large amount of bicarbonate solution has to be used.

 

[Jordan Belfort]

Personally i prefer major neutralisation with baking soda and when it's 5/6 adjust last with lye.

If it's hcl the HCL neutralize to NaCl and gasses, means you already was a part fo your product

 

[Jordan Belfort]

I misread I thought you wanted to adjust pH of the oil after reaction