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

[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.

 

[C14]

This one dont work for pmk powder I tried already

 

[C14]

Hello hcl without water

 

[William Dampier]

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.

 

[C14]

Hello i got one pmk ,people dont said me the cas number but is white powder ,fatty and not shinnig, i tried 2 ways come plastis and floral smell but i dont seee any oil, alcali+acid procees, i listen somes pmk use only hcl acid and not naoh?? Thanks

 

[C14]

Please One question the old pmk can only refluxed wirh hcl, or most use naoh

 

[mixxxman]

just a question to be sure and because i am curious.

the way to the ketone is it the same when is as a powder or oil ?

thank you so much

 

[orgasmatron]

that's a good one. Well, the melting point of it is really low, at around 35-45⁰C you may find it partially melting back and forth making it some weird wax looking mess. The better (powdery) kinds, and now I'm guessing, are probably purer and have a better defined melting point at around 45 deg. When you have mixtures, these properties can vary and unless you are very schooled and experienced at the deed, can be very unpredictable. I haven't seen a third party analysis but it wouldn't make sense to have two different behavior and same substance.
It's one reasonable hypothesis.
Their sales force won't give you a better answer unless you are a lot luckier than me.

cheers

 

[mixxxman]

yes it can be very interesting, to know exactly what it can make the differences between the powder and the oil.
i was thinking, maybe it can be a salt of this molecule, when is as a powder ?
and, if the way can be different between the oil and the powder to the ketone

 

[mixxxman]

if someone can share is knowledge... we are more than happy !
cheers

 

[orgasmatron]

nop. when inquired the very first time about the 'new pmk oil' (CAS 28578-16-7), and asked what would be, if any, the new approach to turn this into real pmk oil ( obviously CAS 4676-39-5) the answer was grand.... "its a trade secret, please don't spread out..." they said. I received a video, it was outstanding! The new product requires just... that you warm it up!... and in the video, I still have it btw, the 'scientist' actually warms up a test tube w/ the solidified product using a lit candle. I was....flabbergasted to say the least. it turns into an oil before your eyes....
I hope we are not talking about the difference between 28578-16-7 and 13605-48-6. This is actually a stable powder and however it produces the same end product if given the right treatment, it is a different molecule altogether and actually gives less yields than it's newer sibling.

Cheers!

 

[PepitoPistol]

Ar
Are you talking about MELTING something??? Wow, I could have never figured out that if you heat a wax it actually melts and turns into an oily thing…
People, please do your research, read, then come here and ask specific questions…
There’s a basic chemistry knowledge required for all this.
Not trying to kick anybody out, but some questions imply that you don’t even understand what a cas number is, what a salt is, etc… It will be (even more) dangerous for you. First step is to do your best to study and learn some basics.
The rest is pretty much already answered in this same thread, again READ before reasking the same over and over.
Just my 2 cents.

Wax/oil and powder are not the same thing, they don’t have the same cas number.
Good luck!

 

[btcboss2022]

Hello,

This is the final stuff that I got from CAS 28578-16-7 wax form:

;-)
Anyway I will test other methods and make some changes to try to improve it as max as possible.

 

[Bartholomeus]

Beautiful crystal, hats off to chemist

 

[Cruela]

Hello guys.
I'm a little confused about which route do l have to do
I have 1 kg of new pmk ( I guess) but I dont know if it's Wax or Powder
When I squeeze the bag it feels like kinetic sand, Not like powder.
The product smell amaizing with this characteristic safrole odoor
But have a spice or acetic odoor, itchy nose

The supplier gave me this instructions:
1- mix this 4 ingredients in this order
Pmk powder, HCL, Water, and Ethanol the Ratio is 1:2:1:1
Test with 100 gr of powder at a time
2- Mix these four ingredients together and stir them well heat at 70-75 degrees and stir for 3 hours containers cannot be completely sealed
3- And then there's the layering. Get rid of the others. Leave the Oil

I think that this metod is for the old version, and I should do the proess that @Fring did.

What would you do?

Thanks for your help.

 

[William Dampier]

The powder looks like the real thing.
Maybe
Excellent. There is always an admixture of finished oil in these products.
quite possible
Yours is more likely a sodium or potassium salt (check for water solubility). The proposed method should work.

 

[little499]

sir,i think this question may be a bit stupid, all because i'm a mewbie,but i want to ask:
how should i make it crystallize if i use the new bmk oil method

 

[masterpell]

I don’t know what the hell my supplier provided me, and the oily substance it produced was surprising.

 

[William Dampier]

you can try to distill or generally understand what the problem is, if you’ve consulted with experts.

 

[C14]

Hello how many hcl ml you used for 100 grams pmk? Thanks

 

[William Dampier]

you can add acid until pH 1-3, and control it during the conversion. Then the question of quantity will be precisely resolved.