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

[Bennyboy88]

Hello freebase:acetone ratio is 1:10, I dont filtered the starting powder what you mean exactly?
Thanks.

btcboss2022With 1:10 ratio. The filtered product should be very clean.

The powder I was referring to is the fine crystal from the freezing actone mixture. Then use these filtered crystal and melt with h20 again. Correct. Thx.

 

[btcboss2022]

With 1:10 ratio. The filtered product should be very clean.

The powder I was referring to is the fine crystal from the freezing actone mixture. Then use these filtered crystal and melt with h20 again. Correct. Thx.

Bennyboy88Hello,

I got very small amount of powder after crystallizing in acetone are mostly big crystal pieces and I filter them yes.

 

[tajira]

Hey did anybody tried [email protected] for PMK? is it reliable?

 

[Zarder]

Hi, so the method described in the beginning of this thread does work? And does one vacuum distill the ketone to purify afterwards? Is this necessary?

 

[Zarder]

What about the enol that remains?

 

[G.Patton]

Hi, so the method described in the beginning of this thread does work? And does one vacuum distill the ketone to purify afterwards? Is this necessary?

ZarderHi, yes, it is still here by reason that it works. Yes, it worth to distill before further synthesis.

 

[Katty Korner]

I think someone asked this, but I didn't see a reply. Can the amount of water be reduced in the initial step, with all other ratios staying the same? And can one use diethyl ether in place of dcm for all uses of dcm here?

 

[btcboss2022]

I think someone asked this, but I didn't see a reply. Can the amount of water be reduced in the initial step, with all other ratios staying the same? And can one use diethyl ether in place of dcm for all uses of dcm here?

Katty KornerHello,

If you reduce the water amount possibly the oil will be less clean about replace DCM by Ether no problem.

 

[Katty Korner]

Hello,

If you reduce the water amount possibly the oil will be less clean about replace DCM by Ether no problem.

btcboss2022Thank you! I doubt I'd ever go at this scale, but I'd probably just clean it up with the bisulfite addiction, I believe that works with ketones.

 

[joejoe]

1. Put 47,5 liters of H2O in the reactor and add 2,5kg of sodium bicarbonate, stirring until complete dissolution, take out the mixture and keep it.

btcboss2022Hello,does put 47 mean is adding aluminum?What is the serving size?

 

[btcboss2022]

Hello,does put 47 mean is adding aluminum?What is the serving size?

joejoeAluminum? I think you are confused with another thread.

 

[Hank Schrader]

For many years we have been engaged in the production of phenylethylamines.
MDMA - high purity and no impurities.
We get the substituted ketone from methyl glycidate.
We use several technologies in the production of MDMA.
The resulting ketone after the hydrolysis of glycidate, we fractionally distill under vacuum.
The purified ketone is mixed with methylamine and dried from the formed water. The resulting imine is reduced to amine.
We select the base and distill fractionally under vacuum.
All substances that are chasing to the desired temperature are discarded. The desired fraction is collected and neutralized in ether with trimethylchlorosilane.
The resulting salt is filtered on centrifuges and washed with chemical grade acetone.
After that, it is filtered again, dried and crystallization is formed on the basis of mixtures of alcohols.
The recovered crystals are washed again with ether to dry quickly.
A cycle of 4 days allows you to get from 50 kg of finished MDMA.
We are always ready to cooperate with manufacturers and wholesale buyers.
We can guarantee the quality of our products and services.

 

[Hank Schrader]

As we can see, 1 cycle I have 31 liters of MD ketone with a total weight of ~ 37.5 kg
The next photo is a filtered MDMA salt.
The next photo is the vacuum drying of an MDMA crystal.
And the crystal after drying.
As a result, we get a snow-white crystal of MDMA hydrochloride with a yield of 40-43KG, which by moles is more than 85-90%+ yield for ketone.

 

[Hank Schrader]

As we can see, 1 cycle I have 31 liters of MD ketone with a total weight of ~ 37.5 kg
The next photo is a filtered MDMA salt.
The next photo is the vacuum drying of an MDMA crystal.
And the crystal after drying.
As a result, we get a snow-white crystal of MDMA hydrochloride with a yield of 40-43KG, which by moles is more than 85-90%+ yield for ketone.

Hank Schrader...

 

[CryptedMind]

Hello,

After check and test the methods posted in the thread http://bbzzzsvqcrqtki6umym6itiixfhn...-methyl-pmk-glycidate-conversion-to-pmk.2013/ I decided the post the best method for me:

1. Put 47,5 liters of H2O in the reactor and add 2,5kg of sodium bicarbonate, stirring until complete dissolution, take out the mixture and keep it.
2. Put in the reactor 7L of H2O
3. Add while stirring 1,2kg of sodium hydroxide
4. While the H2O and the sodium hydroxide are mixing and getting temp put 5kG of wax PMK to melt by low heat.
5. When PMK is melted add it to the reactor and put the mixture at 80 °C reflux during 1 hour stirring.
6. Add 3,25kg of HCL 37% in small portions, once all added keep the mixture at 80 °C reflux during 1 hour stirring.
7. Stop stirring and put the mixture at 25 °C.
8. Discard the water top layer.
9. Put again in the reactor the oil top layer.
10. Add the H2O and sodium bicarbonate mixture, stirring 2-3 minutes.
11. Add 10 liters of DCM (from freezer preferably).
12. Let it get separated around 10-15 min.
13. Evaporate DCM from the bottom layer.

PMK oil (MDP2P; cas 4676-39-5) yield is 3,72kg.

btcboss2022
hello again , just to be sure, i need a more extense explanation in couple points, i was using with success the Fring metod, the one you mention here with a link, and yours there are a thing i need to be sure before to try/loss something, so:

in the finalm step, he just wash with NAOH and the remaining oil is vacuum distilled to get rid of the water in it , but you instead, add DCM, so the question is, i assume thats an extraction in the DCM , then you distill to get pure oil, right? i mean the oil goes to the DCM, a normal extraction?

so the step is , instead to wash with naoh, and discard the water layer, then distill to get rid of water, after you wash with bicarbonate, YOU DONT SEPARATE ANY LAYER? YOU JUST ADD DCM, THEN KEEP THIS DCM LAYER TO DISTILL AFTER? i think i understood, and sounds logicall, but i prefeer to read it from you , please let me know....

 

[btcboss2022]

Hello,

After check and test the methods posted in the thread http://bbzzzsvqcrqtki6umym6itiixfhn...-methyl-pmk-glycidate-conversion-to-pmk.2013/ I decided the post the best method for me:

1. Put 47,5 liters of H2O in the reactor and add 2,5kg of sodium bicarbonate, stirring until complete dissolution, take out the mixture and keep it.
2. Put in the reactor 7L of H2O
3. Add while stirring 1,2kg of sodium hydroxide
4. While the H2O and the sodium hydroxide are mixing and getting temp put 5kG of wax PMK to melt by low heat.
5. When PMK is melted add it to the reactor and put the mixture at 80 °C reflux during 1 hour stirring.
6. Add 3,25kg of HCL 37% in small portions, once all added keep the mixture at 80 °C reflux during 1 hour stirring.
7. Stop stirring and put the mixture at 25 °C.
8. Discard the water top layer.
9. Put again in the reactor the oil top layer.
10. Add the H2O and sodium bicarbonate mixture, stirring 2-3 minutes.
11. Add 10 liters of DCM (from freezer preferably).
12. Let it get separated around 10-15 min.
13. Evaporate DCM from the bottom layer.

PMK oil (MDP2P; cas 4676-39-5) yield is 3,72kg.

btcboss2022

YIELD IMPROVEMENT​

Possibly many people think about it or even do it, in fact I don't know why I don't put it in the process here because I do it each time hahahah

Point 8. "Discard the water top layer" MISTAKE always is remaining oil in the water layer so to improve oil yield we must extract that oil from this layer.

Method:

- Add NaOH+H2O solution to the water layer until PH 12.
- Add DCM to the mixture stir and let separate layers.
- Discard top layer.
- Add the bottom layer to the bottom layer separated in point 12.
- Optional before point 13 you can dry and filter the mixture.

Sorry to forgot to add it before!

 

[J-man]

Hi everyone, sorry but is the starting material here, this PMK wax. Is this just Paraffin Wax, Piperonyl Methyl Ketone PMK? Or is this PMK wax something completely different? Thanks

 

[G.Patton]

Hi everyone, sorry but is the starting material here, this PMK wax. Is this just Paraffin Wax, Piperonyl Methyl Ketone PMK? Or is this PMK wax something completely different? Thanks

J-man

PMK oil synthesys from PMK (CAS 28578-16-7 wax form) large scale​

Hello, there is CAS number in the heading

 

[J-man]

Hello, there is CAS number in the heading

G.Pattoni must be dumb or just blind but im still confused...other than seeing that PMK stands for Piperonyl Methyl Ketone... so thats right, right? PMK oil from PMK wax (Piperonyl Methyl Ketone) same stuff thats in candles and such? Also called Paraffin wax? Is that correct?

​

 

[G.Patton]

i must be dumb or just blind but im still confused...other than seeing that PMK stands for Piperonyl Methyl Ketone... so thats right, right? PMK oil from PMK wax (Piperonyl Methyl Ketone) same stuff thats in candles and such? Also called Paraffin wax? Is that correct?

​

J-manWax form means that this substance looks like wax. It is slang name. There are nothing common with wax from candle, lol.

 

[J-man]

okie dokie, So PMK doesn't stand for Piperonyl Methyl Ketone? Because Piperonyl Methyl Ketone is also called Paraffin and used in candles. Thats how i have made this connection..but i am wrong?

J-manI guess another question would be is PMK glycidate oil the same thing as PMK Piperonyl Methyl Ketone? I have looked but still unsure as there are many answers saying Piperonyl Methyl Ketone is PMK? Thanks

 

[J-man]

I guess another question would be is PMK glycidate oil the same thing as PMK Piperonyl Methyl Ketone? I have looked but still unsure as there are many answers saying Piperonyl Methyl Ketone is PMK? Thanks

J-manNever mind lol, i just worked it out. so, this PMK you start with here- (PMK glycidate oil) is different to PMK Piperonyl Methyl Ketone.. you end up with PMK Piperonyl Methyl Ketone (MDP2P) (4676-39-5) after doing this PMK oil Synthesis!
Haha man.. Good times