反应详情

A mixture of 2-chloro-4-cyano benzoic acid methyl ester (12.4 g, 63.4 mmol) and potassium carbonate (1.3 g, 9.4 mmol) in dimethylsulfoxide (40 mL) was treated dropwise under cooling with 30% hydrogen peroxide (7.6 mL). The mixture was allowed to warm to room temperature and stirred overnight. The solution was quenched with water and the resulting precipitate collected by filtration. The crude material was dissolved in dichloromethane and absorbed on a silica gel Merck-60 flash column. Elution with a dichloromethane-methanol gradient (from 98:2 to 90:10) provided the title compound (10 g) as a white solid, m.p. 154-156° C.

1. additionwas treated dropwise
2. customThe solution was quenched with water
3. filtrationthe resulting precipitate collected by filtration
4. dissolutionThe crude material was dissolved in dichloromethane
5. customabsorbed on a silica gel Merck-60 flash column
6. washElution with a dichloromethane-methanol gradient (from 98:2 to 90:10)