反应详情

温度

80 °C

To a stirred solution of methyl 2-(3-chloro-4-(trifluoromethylsulfonyloxy)-phenyl)acetate (4.419 g, 13.283 mmol) in dimethylformamide were added zinc cyanide (1.6 g, 13.681 mmol) and tetrakis(triphenylphosphine) palladium (1.5 g, 1.3283 mmol). The reaction mixture was stirred for 34 h at 80° C., then cooled to room temperature and diluted with ethyl acetate. The mixture was filtered using celite pad. The filtrate dissolved in ethyl acetate and extracted with NaHCO3. The organic layer was dried over magnesium sulfate and filtered. The filtrate removed in vacuo. The crude was purified by column chromatography to give methyl 2-(3-chloro-4-cyanophenyl)acetate (1.044 g, 37%).

1. temperaturecooled to room temperature
2. filtrationThe mixture was filtered
3. dissolutionThe filtrate dissolved in ethyl acetate
4. extractionextracted with NaHCO3
5. dry with materialThe organic layer was dried over magnesium sulfate
6. filtrationfiltered
7. customThe filtrate removed in vacuo
8. customThe crude was purified by column chromatography