28578-16-7 To mdp2p help

[Handsomerx]

This is so frustrating.
I’ve followed processes to the T and first i yielded a resist clear oil, this second time distilling under vac not exceeding 106c I yielded a totally clear liquid which smells like solvents.
idk anymore.
Here’s some pics of after adding the pmk oil to 300 ml of naOH (16%) heated and stired for. 2hours. Then slowly added h2so4 and oxalic acid and again stired. Added xylene after it cooled and then washed w h20, sodium bicarbonate, and brine, several times
These are pics after adding to sep funnel

 

[LoneChemist]

Hello friend;
Your question is not clear, or your intentions. My understanding is:
CAS 28578-16-7 is PMK Ethyl Glycidate. It commonly comes in form of a powder.
PMK (Piperonyl methyl ketone) is simply a synonym/another name for MDP2P and is always an oil.

after adding the pmk oil to 300 ml of naOH (16%) heated and stired for. 2hours. Then slowly added h2so4 and oxalic acid and again stired

HandsomerxThe above quoted description, were you attempting the hydrolysis on what's already MDP2P?

 

[w2x3f5]

This is so frustrating.
I’ve followed processes to the T and first i yielded a resist clear oil, this second time distilling under vac not exceeding 106c I yielded a totally clear liquid which smells like solvents.
idk anymore.
Here’s some pics of after adding the pmk oil to 300 ml of naOH (16%) heated and stired for. 2hours. Then slowly added h2so4 and oxalic acid and again stired. Added xylene after it cooled and then washed w h20, sodium bicarbonate, and brine, several times
These are pics after adding to sep funnel

Handsomerxmake a small experiment of hydrolysis in phosphoric acid. Your color is disgusting, go wrong.

 

[Handsomerx]

make a small experiment of hydrolysis in phosphoric acid. Your color is disgusting, go wrong.

w2x3f5No it’s pmk ethyl glycidate oil, the above CAS number.
Thanks for th suggestion but I do not have phosphoric acid.
I have a clear red oil now…will try to vac distill it today.

or ill make more.

But are you saying that I could take this pmk ethyl glycidate (purchased from china) and just run it in reductive amination? If so That doesn’t seem correct

 

[UWe9o12jkied91d]

No it’s pmk ethyl glycidate oil, the above CAS number.
Thanks for th suggestion but I do not have phosphoric acid.
I have a clear red oil now…will try to vac distill it today.

or ill make more.

But are you saying that I could take this pmk ethyl glycidate (purchased from china) and just run it in reductive amination? If so That doesn’t seem correct

HandsomerxI dont think it works like that but stranger things have happened.
Anyways MDP2P is a solid at rt, it has a melting point of 88C, atleast from what I have read.

 

[w2x3f5]

No it’s pmk ethyl glycidate oil, the above CAS number.
Thanks for th suggestion but I do not have phosphoric acid.
I have a clear red oil now…will try to vac distill it today.

or ill make more.

But are you saying that I could take this pmk ethyl glycidate (purchased from china) and just run it in reductive amination? If so That doesn’t seem correct

HandsomerxWhere I said it? of course can't, only ketone can use in reductive amination

 

[diogenes]

I dont think it works like that but stranger things have happened.
Anyways MDP2P is a solid at rt, it has a melting point of 88C, atleast from what I have read.

UWe9o12jkied91dMDP2P is liquid, even after storage in the freezer at -20C for about a week.

 

[diogenes]

MDP2P is liquid, even after storage in the freezer at -20C for about a week.

diogenesI distilled the MDP2P under vacuum, boiling point was @190C even with vacuum, but the result was light green and after reduction with MeNH2 in MeOH yielded a beautiful white MDMA crystal (biologically tested).

 

[w2x3f5]

Free idea for you. Three-necked flask + thermometer + dropping funnel + bend / straight condenser / alonge / receiving flask.
Mix in a flask 1 to 1 pmk glycidate and phosphoric acid, heat or a magnetic stirrer or tile and a boiling stone in a flask. Boil for an hour at a temperature of 100+ degrees, control that there would be gas evolution (similar to boiling), after an hour you start adding water dropwise, keeping the temperature above 100 degrees, pure ketone will fly away with hot water vapor. You determine the end of the reaction when the gases stop emitting and the water from the refrigerator will be transparent (not cloudy). Plus, the reaction you have ketone will continuously fly away from the reaction (there is less chance that it will become ill from long heating in hot acid), the second plus immediately pure ketone at the exit.

 

[Cruela]

Free idea for you. Three-necked flask + thermometer + dropping funnel + bend / straight condenser / alonge / receiving flask.
Mix in a flask 1 to 1 pmk glycidate and phosphoric acid, heat or a magnetic stirrer or tile and a boiling stone in a flask. Boil for an hour at a temperature of 100+ degrees, control that there would be gas evolution (similar to boiling), after an hour you start adding water dropwise, keeping the temperature above 100 degrees, pure ketone will fly away with hot water vapor. You determine the end of the reaction when the gases stop emitting and the water from the refrigerator will be transparent (not cloudy). Plus, the reaction you have ketone will continuously fly away from the reaction (there is less chance that it will become ill from long heating in hot acid), the second plus immediately pure ketone at the exit.

w2x3f5This free idea is only for Wax pmk or works in powder pmk?
And then I should distill the Ketone?

 

[w2x3f5]

This free idea is only for Wax pmk or works in powder pmk?
And then I should distill the Ketone?

CruelaIt doesn't matter if it is glycidate or sodium salt, in both cases hydrolysis occurs. Hands did not reach to check on 3.4MD glycidates, it should work similarly to BMK glycidate.

 

[Cruela]

It doesn't matter if it is glycidate or sodium salt, in both cases hydrolysis occurs. Hands did not reach to check on 3.4MD glycidates, it should work similarly to BMK glycidate.

w2x3f5Maybe I ask wrong, I undertood that this method only works with PMK Methyl glicidate actually Banned.
The product that we have is PMK Ethyl glicidate

 

[w2x3f5]

Maybe I ask wrong, I undertood that this method only works with PMK Methyl glicidate actually Banned.
The product that we have is PMK Ethyl glicidate

CruelaI do not have ethyl glycidate, but the factory claims that the hydrolysis technology is similar. Hydrolysis in phosphoric acid also works with Diethyl(phenylacetyl)malonate.
I see no problem for you to try hydrolysis in phosphoric acid on a small amount of substance.

 

[w2x3f5]

Maybe I ask wrong, I undertood that this method only works with PMK Methyl glicidate actually Banned.
The product that we have is PMK Ethyl glicidate

Cruelaread about the Darzan reaction (Darzan condensation)