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

[Gofast]

I’m having the same issue with the wax. After saponification and reaction with HCI a nice light brown coloured oil comes out. After letting this cool off to room temperature it turns dark brown, almost black and thick.

Anyone has input on this?

 

[Bennyboy88]

Try with the no Noah.

 

[Gofast]

Did you already try this? How was your yield?

 

[Bennyboy88]

My fd tell me about 60%

 

[Fring]

it needs final step, vacuum distillation to separate the impurities/water in the brown glue you mention

 

[Fring]

and yes.... the 1 step by rearranging with HCL is not valid with that wax, it needs before (as you can read in this post and in the others) NaoH 5% with dH2o , then hcl, then brine or even better neutralize with Nahc03 and then the vacuum distilation.

 

[HCL]

somebody has an actual tested method that works with a high yield? Talking about cas 28578-16-7

 

[Gofast]

Thanks for your answer. Maybe I was unclear but what I meant was that I did it in 2 steps. First naoh (and let it sit for at least one hour) and after that the reaction with HCL. Where after adding the the HCL it separated in to two layers.

With the old powders I never distilled them and was able to always use it the oil perfectly fine.

Are your results getting better with the above methods?

 

[Fring]

in fact the problem is when we compare with the old pmk , because when we obtain that weird organic layer we think all failed , then we dont go ahead, but as i knew everybody who followed the base/acid method had to distill... i would love to know the results if someone follows the hydrogen peroxide method i published in my opened post, because it seems will be much more perfect and clear, but im not willing to handle hydrogen peroxide at more than 70% without a PRO fume hood... i have an extraction aparatus , but.. i'll not take that risk, anyway this method was sent to me from the big form the manufacturer of the stuff, not the re-sellers..so it should be the best of the best options.

 

[Fring]

Well...after some fails, i think i have done finally... thee result are clean oil, no dirty stuff..no more honey look, but with a big difference if we compare with methyl pmk, the result colour is an brown-dark red oil, with an intense sassafras smell which keeps the state in room temp, and never get freezed, the key id VaCUUM DISTILLATION, dont need a lot of distillation, the water in the post-distillation product its just a little bit.
if you do you will see pretty soon that the reaction is done... no more water passing thru condenser and only a reflux of the oil happens. i will upload pics if i find a comfortable method to do it here.

 

[ASheSChem]

the forum is safe

 

[Gofast]

Well...after some fails, i think i have done finally... thee result are clean oil, no dirty stuff..no more honey look, but with a big difference if we compare with methyl pmk, the result colour is an brown-dark red oil, with an intense sassafras smell which keeps the state in room temp, and never get freezed, the key id VaCUUM DISTILLATION, dont need a lot of distillation, the water in the post-distillation product its just a little bit.

 

[Gofast]

Congratulations on that! Would you mind on sharing the exact recipe and steps used?

 

[Fring]

 

[Fring]

Sure!

1st of all, sorry for my English, i know can be" weird" sometimes..

so, i tried different quantities on the base-acid method till i found the correct.
THE KEY ANYWAY IS THE VACUUM DISTILLATION, i write on Capital because ive seen that (same as happened with me at the beggining) after do the base-acid, whe we see the result (a dirty and extreme dense crappy honey) we think something was wrong , then we dont go ahead.. but here is the key.
FOR 50 GR OF WAX ( went low scale because i have just a small amount of wax)

1. put the 50 gr wax and 70 ml dH2O and 12 Gr Lye , slowly increase the temp at 80º C , when the 80º reached keep stirring it for one hour.

2. add to the mix 32,5 gr of HCL 65% and keep stirring for 1 hour more at 80ºC

3. put in Sep funnel , discard the water layer and add a decent amount of dH2o with 5% sodium bicarbonate (or just make a saturated solution) and do the typical operation in sep. funnel and let it sit for 30 minutes

4. repeat 2 x more times the saturated solution washing, discard water always and the 1 only water washing.
( if an emulsion appears try brine wash)...

5. vacuum distill till all water goes (its just a small quanty who are giving the problems) and could be done in rotovap.
and....

VOILA! you have the desired product, just with a different colour than the old glycidate gaves... the result will be a dark red-brown oil.

 

[justlooking88]

Can somebody explain the difference between these 2 cas numbers regarding pmk? one seems to be pmk ethyl glycidate and the other pmk methyl glycidate , which is considered old one which converts easily and which is the new one everybody is having a hard time with? Any help would be amazing

13605-48-6 pmk methyl glycidate

vs

28578-16-7 pmk ethyl glycidate

 

[malayboy]

hi @Fring, I would like to know as well, the exact CAS number of Ethyl-Methyl Glycidate for this crucial MDMA precursor, PMK(MDP2P) synthesis
@G.Patton @William Dampier

 

[Fring]

dont loss your time man , trust me the Chinese are ALL selling the ETHY METHYL form since the ethyl is banned, they dont play when something is banned..they can sey what they want, but its all ethyl, maybe they even dont know... bear in mind that the vast majority of them dont know nothing about it, they just sell it.

 

[mixxxman]

just a question by the way someone can explain to me the difference of the powder and the wax ?
cause with a chemistry mind, i don't relly understand the difference of this 2 form.
what exactly change ? the bolting point is not the same ? one is more like a "salt" and the other one is a different texture but with the same molecule ?
all of these details confuse me and i don't really understand.
and if also, if all of these kind of precursor need the same conversion to be a ketone.
thank you for your informations

 

[Montecristo]

thanks for that write up! i take it you mean 35% HCl ?