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

[Montecristo]

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.

Fringwhat yield did you get in the end?

 

[mixxxman]

someone can explain to me the difference on the molecul when it's powder or vax ?
why is like that, and when i am asking directly to them.... they don't have a real answer.
as a chemist mind... i really to understand everything.

and ok, the pmk glycidate was banned / ok the pmk methyl glycidate is banned / right to be clear we have only the PMK ETHYL GLYCIDATE.

someone knows the difference on the conversion ? or if this new group bring something different to the yield at the end.
i am curious to get some tips and differents point of view.

and i have the feeling the kind of oil we have at the end it's bit crappy..

someone has some technique to have a best oil, very clear and pure or doesn't matter during process ?
thank you

 

[orgasmatron]

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.

Bennyboy88maybe this can sound annoying or excessively stupid of me, or maybe its the loose definitions thrown around all the time. When you guys say "the one that is solid", does that mean CAS 13605-48-6 or the 28578-16-7 in alleged "powder" form, and is there such thing? What do the chinese mean by powder 28578-16-7? It is my noob preconception that if there is a substance, it has it's own cas, if there is some salt of it, it's a different CAS.
So at the end of the day I would finally like to know what would the best procedure for CAS 13605-48-6 be? If it is the procedure previously described and referred to the Sydney bust, how can one optimize the maximum total volume in the flood ( for 35g, the paper indicates 600ml flood, very unpractical and troublesome)? And how can the copper step from the procedurebe skipped (using hcl?)
thanks everyone

 

[mixxxman]

and by the way, because... it sound right now most of the mdp2p from this new pmk glycidate it make me a dark and not very clear oil...
some people have few tips ?
cause i would like to know, after the conversion what is the best to extract this ketone.
which kind of solvent can i use to clean my oil ?
few method to make it more clear and pure ? ( distillation ? freezer ? washing with saturated nahco3 ?

 

[Fring]

and by the way, because... it sound right now most of the mdp2p from this new pmk glycidate it make me a dark and not very clear oil...
some people have few tips ?
cause i would like to know, after the conversion what is the best to extract this ketone.
which kind of solvent can i use to clean my oil ?
few method to make it more clear and pure ? ( distillation ? freezer ? washing with saturated nahco3 ?

mixxxmanwhy you all guys want to have a non dark oil? whats the matter? this is different pre-precursor, so the result is different...dark red oil... the goal is to have a clean and non dirty oil, following the descibed method (base-acid) the vacuum distill... the result is DIFFERENT, not the same GLY as before guys... so not the same colour...

 

[PepitoPistol]

why you all guys want to have a non dark oil? whats the matter? this is different pre-precursor, so the result is different...dark red oil... the goal is to have a clean and non dirty oil, following the descibed method (base-acid) the vacuum distill... the result is DIFFERENT, not the same GLY as before guys... so not the same colour...

FringVisual aspect of a substance is characteristic of it, if there is a notable difference then it might mean it has high amount of contaminants. Do you vacuum distill the ketone? Or just remove the water?
I’m waiting for some PMK ethyl gly…

 

[Darkie1990]

As i was reading all topics about the PMK-glycidate with CAS: 28578-16-7 to be clear it can come in powder and in oil substance which can get hard under 33*C. All methods above is about the oil/wax substance.

As far as i could get notes about the process i write it in clear language so people can understand this better (included me). I have some questions about those improvements and what to do if made so.

Step one:
Mix 1.4 LT DH2O (distilled water) and 240 gr NaOH (Sodium Hydroxide, lye, caustic soda.) and 1 kg eth-gly-pmk cas:28578-16-7 at 80º for an hour

Improvement as read at the forum:

Instead of mixing distillated water with NaOH and pmk-gly-eth at 80*C for an hour we now mix this at a temperature of 20-21*C for 12 hours.

Question about the improvement:
Do we heat this up to 80*C or do we keep it with NaOH at 20*C. Do we add PMK-gly-eth at 20*C directly or we heat more up?

Step 2: adding acid:

Add 650g HCL 65%, hydrochloric acid, at 80º mix an hour.
2. Concentrated HCL , next time i'll add dropwise till end of bubbling/visible reaction and measuring PH-3

If improvement was made in the step with NaOH and we are adding hydrochloric acid do we raise temperature to 80*C? or do we keep it at 20-21*C? if keep it at 20-21*C do we continue again 12 hours or do we add this step within the first 12 hours?

Step 3 separation:

Put it in separator 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 separator funnel and let it sit for 30 minutes.

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

Step 4 vacuum distill:

vacuum distill till all water goes (it’s just a small quantity who are giving the problems) and could be done in rotavapor.

 

[IM BATMAN]

As i was reading all topics about the PMK-glycidate with CAS: 28578-16-7 to be clear it can come in powder and in oil substance which can get hard under 33*C. All methods above is about the oil/wax substance.

As far as i could get notes about the process i write it in clear language so people can understand this better (included me). I have some questions about those improvements and what to do if made so.



Improvement as read at the forum:


Question about the improvement:
Do we heat this up to 80*C or do we keep it with NaOH at 20*C. Do we add PMK-gly-eth at 20*C directly or we heat more up?

Step 2: adding acid:


If improvement was made in the step with NaOH and we are adding hydrochloric acid do we raise temperature to 80*C? or do we keep it at 20-21*C? if keep it at 20-21*C do we continue again 12 hours or do we add this step within the first 12 hours?

Step 3 separation:




Step 4 vacuum distill:

Darkie1990well...didnt tried the saponification at room temp. for 12 hours, but i will for sure, since the dark brown colour in this conversion appears after the 80c saponification..maybe it can solve it...about other benefits i dont know....

as for the acid adittion, thats other proccess, yes you should put at 80ª for sure

 

[IM BATMAN]

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

mixxxmanwell...the mistake here its because some folks thinks they can buy the old CAS , but thats not correct, the only available form is the waxy one, there arr 2 presentations of this , but its just the way the producer are finishing it..one is more yellow wax , and other is more white powder, but as soon as those reach 30ªc they will melt...its the same molecule, trust me.

 

[IM BATMAN]

someone can explain to me the difference on the molecul when it's powder or vax ?
why is like that, and when i am asking directly to them.... they don't have a real answer.
as a chemist mind... i really to understand everything.

and ok, the pmk glycidate was banned / ok the pmk methyl glycidate is banned / right to be clear we have only the PMK ETHYL GLYCIDATE.

someone knows the difference on the conversion ? or if this new group bring something different to the yield at the end.
i am curious to get some tips and differents point of view.

and i have the feeling the kind of oil we have at the end it's bit crappy..

someone has some technique to have a best oil, very clear and pure or doesn't matter during process ?
thank you

mixxxmansame products, same proccess...
the matter of improve colour...well..maybe it exists but IMO all the new MDMA will be darker thatn before, you'll see...the new MDP2P is the same stuff but with a darker colour, then the MDMA will darker... just a bit , my results were like old unwashed "coca-cola" looking... no matter how much times you wash it, it keeps that colour

 

[moneyboy888]

As i was reading all topics about the PMK-glycidate with CAS: 28578-16-7 to be clear it can come in powder and in oil substance which can get hard under 33*C. All methods above is about the oil/wax substance.

As far as i could get notes about the process i write it in clear language so people can understand this better (included me). I have some questions about those improvements and what to do if made so.



Improvement as read at the forum:


Question about the improvement:
Do we heat this up to 80*C or do we keep it with NaOH at 20*C. Do we add PMK-gly-eth at 20*C directly or we heat more up?

Step 2: adding acid:


If improvement was made in the step with NaOH and we are adding hydrochloric acid do we raise temperature to 80*C? or do we keep it at 20-21*C? if keep it at 20-21*C do we continue again 12 hours or do we add this step within the first 12 hours?

Step 3 separation:




Step 4 vacuum distill:

Darkie1990

 

[moneyboy888]

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.

btcboss2022

bro can you send me the oil methods,thx

 

[moneyboy888]

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

malayboy
sir , i already have pmk oil
what next step i can do?

 

[malayboy]

sir , i already have pmk oil
what next step i can do?

moneyboy888I am not an expert here, please contact @G.Patton @William Dampier , they are expert in this forum and very helpful

and please make sure your PMK cas no. is correct before proceeding any steps, here is few helpful links you might need to refer:

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/synthesis-of-3-4-methylendioxybenzylmethylketone-from-piperonal-glycide-ester-route-small-scale.24/

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/synthesis-of-mdma-from-piperonylmethylketone-pmk-with-formamide-and-lah.49/

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/threads/need-help-with-pmk-ethyl-glycidate-to-mdma-synthesis.682/

 

[Bartholomeus]

Anyone really producing finished mdma from this new pmk ethyl glycidate succesfully?

Or are everyone just having problems with conversions and not properly able to crystalize the finished product?

Why are there no updates for correct PMK ETHYL GLYCIDATE conversion method?

 

[IM BATMAN]

Anyone really producing finished mdma from this new pmk ethyl glycidate succesfully?

Or are everyone just having problems with conversions and not properly able to crystalize the finished product?

Why are there no updates for correct PMK ETHYL GLYCIDATE conversion method?

ChingShihread better bro, the correct conversion its already posted, and yes, i have beautiful crystals , very small scale, but that will not make difference.

 

[WillD]

Conversion by alkali or acid. If a dirty product, purify with bisulfite adduct (soon video). If all this does not work, then your glycidate is trash.

 

[IM BATMAN]

Conversion by alkali or acid. If a dirty product, purify with bisulfite adduct (soon video). If all this does not work, then your glycidate is trash.

William Dampiercant wait to see the video!!!

 

[Bartholomeus]

Can somebody please write down conversion for 1kg pmk ethyl glycidate?
But only those who tried the conversion and have experience, please don't post copy paste if you aren't sure it works

 

[Octopusssss]

maybe this can sound annoying or excessively stupid of me, or maybe its the loose definitions thrown around all the time. When you guys say "the one that is solid", does that mean CAS 13605-48-6 or the 28578-16-7 in alleged "powder" form, and is there such thing? What do the chinese mean by powder 28578-16-7? It is my noob preconception that if there is a substance, it has it's own cas, if there is some salt of it, it's a different CAS.
So at the end of the day I would finally like to know what would the best procedure for CAS 13605-48-6 be? If it is the procedure previously described and referred to the Sydney bust, how can one optimize the maximum total volume in the flood ( for 35g, the paper indicates 600ml flood, very unpractical and troublesome)? And how can the copper step from the procedurebe skipped (using hcl?)
thanks everyone

orgasmatronI buy from chinese in nowember and december 2021 few kilo of what they told me was CAS 13605-48-6. They didnt deliver any instruction. So what i understand from BenyBoy i should do as below:

The method was provided for the one that is solid at room temp (mine is white powder)

1:1:1 PMK powder CAS 13605-48-6 :etanol : dh20 - heat at 60c for 1 hr
2. Add HCL heat 3.5 hr. At 75c (how much of HCL?) - can somebody give advice?

I ask because there is chance that i have old stuff thay they deliver in late 2021. If its impossible and i have the 28578-16-7 than i will do as it was in this post.

Is there any chance to tell the diference between 13605-48-6 and 28578-16-7 when its in the form of white powder?

Thank You