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

[Curiousonion]

Sorry, meant to say the white powder form.
So there are 3 forms, wax, oil and powder?

 

[btcboss2022]

Pure and clean one is transparent.

 

[btcboss2022]

2 I think, wax and powder and both get oily heating at low temp.

 

[JJRLL]

Thanks

 

[btcboss2022]

IF
If you followed the process step by step you should have 2 layers, explain me point by point what you do exactly

 

[Curiousonion]

Added h20 with distilled water, while it was warming up melted the powder then added it.
Refluxed for an hour, then added hcl and refluxed for another hour.
Stopped reaction, waited for it to cool and seperate.
No separation occurred.

 

[btcboss2022]

H20 with distilled water?;-)
I Guess is a writing mistake you woukd mean NaOH.
What PH has your mixture now?Seems not enough HCL.

 

[Curiousonion]

Yeah sorry, Naoh.
I added the exact amount of hcl as written in the procedure.
Once you add the hcl is start boiling and fuming and when you reach the hcl saturation levels the reaction just settles and changes color to yellowish.

 

[btcboss2022]

What is the current PH?

 

[Curiousonion]

that I don't know anymore, I did that workup last night and neutralized the acid.
What is the ph supposed to be?
I mixed the reaction with a bicarb solution then seperated it with dcm. That seems to work, dcm with oil goes to the top for some reason.

 

[Curiousonion]

I will try another reaction now, what is the ph of the final solution after it cools down to 25c supposed to be?

 

[btcboss2022]

Is not only about neutralize the acid is about to turns the mixture acid.PH after HCL process must be at least in 2. DCM goes to top?Something is wrong for sure now web must Discover what is.
I did that synth yesterday again and allí smooth like always.

 

[Curiousonion]

Ok so I will try it again.
But I followed the exact procedure you wrote.
The dcm with oil in it has that smell that mdma usually has.
I also find it strange that the dcm goes to the top

 

[Curiousonion]

UPDATE:
Tried it again at same ratios provided in original recipe for 333 grams pmk powder.
All ingredients were scaled down.
Upon adding the HCL to the reflux, waited another half an hour, measures ph, it was slightly above 2.
Added more hcl until ph was at 2.
Ended reflux, clear separation occurred.

 

[Curiousonion]

One question, when the 2 layers seperate the oil looks very nice and clean.
Is the bicarb wash that really necessary? Can't the oil be used as such and impurities washed away when doing crystallization at the end?

 

[Bartholomeus]

How did you get such big rocks of crystal? buchner funnel with vaccuum so the crystals get pressed?
And what was your yield from 1L of mdp2p oil to mdma hcl, how many dried Cola mdma crystals you got from 1l mdp2p?
If you maybe know the dry yield already

 

[btcboss2022]

In my opinion is necessary because is not only about impurities the final mixture is too acid so is not good idea to use it directly, the bicarbonate-water washing will remove part of that acid and any future process will be smoother.

 

[btcboss2022]

The crystals are made with normal crystallization process first with acetone and later with water you can find a lot of different techniques for that.
From 1L I got around 900gr.

 

[btcboss2022]

UPDATE:

In big scale step 6 must be done in cold, is very dangerous and slow to make that step in hot.

 

[yin-yang]

I thought refluxing it with HCl was enough. I know it would work with methyl glycidate, but what about ethyl? Is this krapcho decarboxylation?