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....