All in One Thread for Ethyl-Methyl PMK Glycidate conversion to PMK

[Fring]

Since it seems a lot of folks (including me) are having problems with the conversion / re-arrangement of this "new" pmk glycidate, i think we could put toguether all in thus thread to see if we finally get a 100% working conversion recipe.

im following an Alkali-hcl with NaHCO3 washing with bad results, dense and dirty dark brown olily substance.
but i have a very new Way , that ill post at the end of this thread, sound very interesting, but first what i tried and failed:

1: dH2o with NAOH , and the GLYCIDATE for 1 HOUR AT 80º
2. Concentrated HCL , i think im using a lot, next time i'll add dropwise till end of bubbling/visible reaction and measuring PH-3
3. DISCARD aqueous (maybe should i do the NAOH 5% washing before discanding? )
4. the NAOH washig , if still visible aqueous , Brine
5. 2 water wash till the water in contact with the organic layer shows neutral PH
and the result is that dense dirty crap..... any idea? advices?


the new and promising conversion i received:

1. put the wax and hydrogen peroxide in a ratio 1:8 (what purity of HP? DONT KNOW)
2. Heat, slowly add acid dropwise while stirring and controling PH value (no more info, i suppose till reach 3 or so)
3.after reaction compelted for 2 hours the reaction liquid is extracted with hydroxide sodium solution (i suppose 5%) and the water phase is obtained
4.. the obtained water phase is then added dropwise with acid to adjust the ph value untill an oily substance appears, and the oily substance is extracted with an organic solvent, and then evaporated TO OBTAIN IT

sound very good isn't? but i dont know the safety advices for handle high concentration hydrogen peroxide, never used it...any suggestion?
soince they dont let know what concentration of HYDROGEN PEROXIDE should i use , i suppose the higher possible..here i can find with a lot of difficult 70%

any thoughts?

i only have 100 grams of the ETHYL GLYCIDATE, so i cant loss more trying all..... im trying this synth as a personal satisfaction...

 

[btcboss2022]

What CAS are you talking about exactly?
Thanks.

 

[Fring]

Not remember now, im not at home, but the new one, the waxy ethyl.methyl pmk glycidate, the one which is giving problems to everyone, unless we find the solution here

 

[btcboss2022]

I have methods for CAS 28578.

 

[Fring]

this is the oil or the white powder form right?
the problem comes with the waxy one..but i have access to the white powder version, could you please send me the method? ill be very grateful with you.
tnx!

 

[btcboss2022]

Oil, I have methods but not done myself yet I'm waiting an order once I prefer to make them I share the results with all experience on it.
Thanks.

 

[Fring]

It seems that the oil only needs direct rearrangement with HCL, same as the old pmk Gly..... then lets see how it goes and please, remember to post here..tnx mate!

 

[btcboss2022]

The info that I have is not this way I will update you.

 

[Selassi]

I have heard for this new gly the recipe was just with Ethanol, Water and HCl?

 

[btcboss2022]

My advice is forgot all literature synth posted that is not done personally and wait that we find the best method once we receive the product becasue we have the methods to test directly from producers. Thanks.

 

[Fring]

the second recipe i posted came directly from the producer lab , in fact sounds very logic and promising, but the first method 8alkali-acid) we all know comes from the recipe of one of the customers of my seller... anyway..didnt worked.. and the more PRO method i didnt tested due to difficult acquiring high % hydrogen peroxide...so im at the begginig point..... lets see how it goes with you mate , looking forward to it.
good luck

 

[Fring]

this is the logic and general reaction for esthers and if that supposed "glycidate" would be just that it would work for we all...but there is something weird on it..god knows what they added to avoid legal issues..

 

[malayboy]

I was just decided to open a new thread because of this PMK-Ethyl Glycidate Synthesis route confusion, but you already did

DISCLAIMER: ALL INFORMATION WRITTEN ARE MY PERSONAL INFO GATHERING, THESE ARE POSTED FOR EASY REFERENCING ONLY

As a newbie chemist I believe many folks would run into the confusion like me, so I would just bump everything I found on this forum and info I could, as I did not run experiment at current time, just info gathering, further editing might be held

CAS 28578-16-7, All of the pros are talking about, don't bother the name (PMK-Ethyl Glycidate / BMK-Methyl / Ethyl-Methyl PMK / glycidyl ester)

Here is the link of @Jack mentioned in most of the threads for final MDMA Synthesis

Sci-Hub | Methyl 3-[3′,4′-(methylenedioxy)phenyl]-2-methyl glycidate: An Ecstasy Precursor Seized in Sydney, Australia | 10.1111/j.1556-4029.2007.00480.x

A precursor to a precursor has been simplified a lot by @William Dampier

Synthesis of 3,4-methylendioxybenzylmethylketone from piperonal (glycide ester route)(small scale)

Step 1. PMK-glycidate. 1. Freshly prepared powdered sodium ethoxide (23 g.) was added during 4 hours to a stirred mixture of piperonal (50 g.) and ethyl a-bromopropionate (61 g.), cooled in ice-salt. 2. Stirring was continued overnight at room temperature and for 6 hours on the water-bath...

chemforum.info

If you cannot get CAS 28578-16-7 directly, follow the step of @William Dampier with preparations of
- Sodium Ethoxide CAS 141-52-6
- Piperonal CAS 120-57-0,
- Ethyl a-bromopropionate CAS 30365-54-9
- etc.

CAS 28578-16-7 itself can be in different state and color (Pmk/BMK Oil/PMK White Powder)

i believed the steps was to produce MDMA, although there are various names of MDMA like 3,4-Methylenedioxymethamphetamine

and then the chemical symbols
CAS 20320-59-6
CAS 5413-05-8
CAS 236117-38-7
CAS 28578-16-7

I found out all of these are meth-alike, my guess is all these could be precusor to methamphetamine as well, we just lack of knowledge and experience. Credits to @Jack , @William Dampier , @DocX and @G.Patton , study basic chem and ELI5 to google

 

[Fring]

the problem is that the document of the seized stuff in australia etc, which i already studied, is for the methyl-pmk, (the old an easy to rearrange) not the actual ethyl-methyl form....
in fact the australian equipe followed the old recipe that appears as well in strike total synthesis etc...that cant be used in the new form...
im right @William Dampier ?

 

[Bennyboy88]

The method was provided for the one that is solid at room temp

1:1:1 P:ethonal:dh20 heat at 60c for 1 hr
2 HCL heat 3.5 hr. At 75c

Around 60%

I think there can be improvement.

 

[Selassi]

Yes this is exactly the one i meant

 

[Fring]

those could work for the same CAS, but in oil or powder form, the more common wax need 2 steps, first alkali the acid.... and of course vacuum distillation.

 

[Bennyboy88]

Can anyone else offer there method or input for a higher percentage return.

 

[Bennyboy88]

I'm referring to the that is oil form at over 33c and start to turn into like dry honey at room temp. It this what u mean by the wax stuff. Thx

 

[Fring]

then dont follow the recipe you commented, it will not work.... for the wax you mention you need to 2 alkali-acid-purification, but even knowing it im not having good results...still working on it, changing temperatures, quatity of hcl etc, and seen changes but still bad...