PMK glycidate problems

[CharmingKid]

Hi everyone,
So I have a problem with the wax pmk (cas 28578): I tried to make PMK from it a few times in the alkali- acid method: I first put the glycidate in water with NaOH solution (until the pH was between 8-12) and let it stir for at least 1 hour, than I added HCl until the pH was 4-6 and let it stir for another hour. after that I washed the solution with brine and DCM, evaporated the DCM and I got 2 different results from 2 state of matter:
when I started with liquid PMK glycidate I got after the evaporation some dark crap and when I tried to vacuum distill it I got some red solution that I assumed hat is not pmk- because there is too much difference in colors (picture of that in the right).
when I started with partly solid PMK glycidate I got in the end yellow solution (I didn't do vacuum distillation this time) but I a not sure that I got PMK in this way, because as much as I know- there is another step of vacuum distillation with this PMK (pictures of that in the left)
Any thoughts? What else can I do to get PMK?

 

[Curiousonion]

Why do you think its not pmk exactly?
How much powder did you start with and how much oil you had at the end?

 

[CharmingKid]

Why do you think its not pmk exactly?
How much powder did you start with and how much oil you had at the end?

Curiousonionit not the color, its not the same frezzing point, thats why i thing its not it.

i started with oil/wax,the new one, not powder.
the yeild was 80%

 

[Curiousonion]

When you added the hcl and let it cool did it seperate?

 

[CharmingKid]

yes

 

[Curiousonion]

Then you should wash it with a bicarb solution then extract with dcm.
It should be what you are looking for

 

[CharmingKid]

Then you should wash it with a bicarb solution then extract with dcm.

CuriousonionOk, I had PMK that I washed with brine and extracted with DCM, and when I washed it with sodium bicarbonate it got the right color and texture.
Could it be? can I wash it with brine and DCM and then with sodium bicarbonate and still get what I need?

 

[Curiousonion]

Yes,once it's mixed with the dcm you can wash it with bicarb solution.
What color is it exactly?

 

[Curiousonion]

Also what texture are you referring to? It should be like a syropy oil

 

[CharmingKid]

looks almost legit now! thank you!

 

[CharmingKid]

Also what texture are you referring to? It should be like a syropy oil

Curiousonionok see the attached files.
this is how it looks like and yes the texture is syrop oil.
the color feels right.
after a little beat of heating the oil got clear and see-through.

but after this we tried to distillate this but its only got darker and darker

 

[Curiousonion]

It's ok that it's dark. That's how the new pmk is.

 

[CharmingKid]

It's ok that it's dark. That's how the new pmk is.

Curiousonion
finally some answers... thank you very much my friend, its been driving me crazy.
should i keep it green/yellow color?
and if i heat this and make it darker, does it affect the color of the final product?

 

[Curiousonion]

Why are you heating it?
Best way to do it is to let it separate then do a couple of bicarb washes and afterwards a gentle vacuum distillation to remove the trace amounts of water

And yes, if it is too dark then it will affect the final color of the product but to get it too dark you basically need to overheat it while it still has some acid in it. (It causes oxidation).
But color of new pmk is reddish brownish