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4-methoxyphenyl methacrylate synthesis

3synthesis methods
-

Yield:10430-85-0 82%

Reaction Conditions:

with triethylamine in 2-methoxy-2-methylpropane at 50; for 10 h;

Steps:

5

General procedure: Methanesulfonyl chloride (114.6 g, 1.0 mol), methacrylic acid (172.3 g, 2.0 mol), and ethyl acetate (EA, 200 ml) were added to a 2 L reactor. Then, triethylamine (204.5 g, 2.02 mol) was added while stirring at 0°C. After stirring at room temperature for 3 hours, it was monitored by NMR or GC to confirm whether methacrylic anhydride was synthesized. When the synthesis of methacrylic anhydride was completed, phenol (103.6 g, 1.1 mol) was dissolved in ethyl acetate (110 ml), and then added to the mixture. Then, triethylamine (103.3 g, 1.02 mol) was added and stirred at 50° C. for 10 hours. After confirming the completion of the reaction by NMR or GC, it was filtered using ethyl acetate (450 ml), and the ethyl acetate was distilled off. The mixture was decanted three times with hexane (300 ml), and then the hexane was washed with 5 wt% NaOH aqueous solution (500 ml). The hexane layer was further washed with acetonitrile (60 ml), and the hexane was distilled off to prepare purified methacrylic acid phenyl ester.

References:

KR2022/73424,2022,A Location in patent:Paragraph 0083-0084; 0096-0097; 0122