反应详情

3,4-Dichlorophenol (110 mg, 0.67 mmol) and potassium carbonate (20 mg, 1.42 mmol) were stirred in dimethylsulfoxide (20 mL). After 5 minutes, 4-methylphenyl 5-chloro-2,4-difluorobenzoate (Preparation 10, 200 mg, 0.71 mmol) was added and the reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and washed with a 1M aqueous solution of sodium hydroxide. The aqueous phase was extracted with ethyl acetate. The combined organic phase was dried over magnesium sulphate, filtered and concentrated in vacuo to give a white solid. The solid was purified by silica gel column chromatography (50% ethyl acetate in heptane elution) to afford the title compound as a white solid (286 mg, 95%).

1. washwashed with a 1M aqueous solution of sodium hydroxide
2. extractionThe aqueous phase was extracted with ethyl acetate
3. dry with materialThe combined organic phase was dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customto give a white solid
7. customThe solid was purified by silica gel column chromatography (50% ethyl acetate in heptane elution)