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Author: Subject: BMK Glycidate hydrolyzed decarboxylation problem
pavlik06
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[*] posted on 1-12-2018 at 13:56
BMK Glycidate hydrolyzed decarboxylation problem


Hello, please help. I got from a friend several gram bmk glycidate Benzeneacetic acid CAS: 16648-44-5
Me try experiment to hydrolyze GLYCIDATE to the oil.
This is the procedure I followed.
1,1kg powder mix with 1kg warm water (around 80 degrees).
2, put in 1kg hydrochloric acid (HCL 37%) and you will see bubble generated.
3,Stirring the mixture for one hour and then stop.
4,After one more hour you will get oil layer in light yellow color.
5,Use separatory funnel to retrieve oil.

I proceeded so that after mixing the raw materials I warmed everything to 90-95 C at medium speeds of stirring for two
hours. After hydrolysis and decarboxylation, I collected the top layer and the bottom (aqueous) was extracted twice with
DCM. I mixed the extracts thoroughly with the oil and then washed with water then soda bicarbonate again with water and
then with brine. The purified oil was dried with MgSO4, the solvent was distilled off, and a slightly yellow oil was left as a residue.

I know the problem is in the cleanliness of the oil because in the imine formation the mixture was colored to pink-red.I think the problem that has probably occurred is that unreacted hydrochloric acid remains in the oil because I did not clean the oil with sodium hydroxide solution . Or it could be a problem that I polymerized the oil because I had a wrongly set high temperature above 100C when I was solvent distillation (DCM)

What is your point of view where the problem arose?
Thank you for your reply
Sorry for my English (translator)
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j_sum1
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[*] posted on 1-12-2018 at 16:25


It seems to me that you are seeking a recipe for phenylacetone.
Not happening here.
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1-12-2018 at 16:26

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