Question regarding PMK
- Thread starter Montecristo
- Start date
Methyl, ethyl, tert-butyl, isopropyl, etc. ethers react with alkali and after react with acid. The reaction is always typical for any ether. A big question about the quality of the most glycide ether.
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ran across this synth process for glycidate and was wondering if anyone tried it
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Put glycidate into warm water, add lye until the PH is decently basic.
Stir for an hour to finish the saponification.
Drip in HCl slowly, the solution will bubble. Add it in until the solution stops bubbling and the PH is slightly acidic. (probably don't want it to be too acidic, might break something down/cause polymerization)Stir this for an hour, heated to around 80C.
At this point, the converstion is complete. Extract with DCM, wash DCM with NaCl brine, and evaporate DCM. Bam, you have your final product, ready for vacuum distillation"
"
Put glycidate into warm water, add lye until the PH is decently basic.
Stir for an hour to finish the saponification.
Drip in HCl slowly, the solution will bubble. Add it in until the solution stops bubbling and the PH is slightly acidic. (probably don't want it to be too acidic, might break something down/cause polymerization)Stir this for an hour, heated to around 80C.
At this point, the converstion is complete. Extract with DCM, wash DCM with NaCl brine, and evaporate DCM. Bam, you have your final product, ready for vacuum distillation"
Only for ether, not for salt
The reaction time will depend on temperature and quantity. Better at room temperature and 12 hours or more.
pH<=3, 80-90*C. If there was no excess alkali before, then there will be no strong bubbling at the beginning.
If we have a concentrated aqueous solution (acidic with alkaline salts), and a hot mixture, BMK will be a layer on top.
The reaction time will depend on temperature and quantity. Better at room temperature and 12 hours or more.
pH<=3, 80-90*C. If there was no excess alkali before, then there will be no strong bubbling at the beginning.
If we have a concentrated aqueous solution (acidic with alkaline salts), and a hot mixture, BMK will be a layer on top.
