反应详情

温度

100 °C

A solution of 3-fluoroisonicotinaldehyde (0.25 mL) in dimethyl sulfoxide (2.0 mL) was treated with a solution of 4-fluorobenzene sulfinic acid sodium salt (0.5 g) in dimethyl sulfoxide (3.0 mL), and the resulting mixture was stirred at 100° C. for 3 days. The mixture was cooled to room temperature, partitioned between water and ethyl acetate (20 mL), and the aqueous phase extracted with ethyl acetate. The combined organic solution was dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with a mixture of dichloromethane and ethyl acetate (1:0 to 4:1 by volume) to afford the title compound as a white solid (0.38 g).

1. temperatureThe mixture was cooled to room temperature
2. custompartitioned between water and ethyl acetate (20 mL)
3. extractionthe aqueous phase extracted with ethyl acetate
4. dry with materialThe combined organic solution was dried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel
7. washeluting with a mixture of dichloromethane and ethyl acetate (1:0 to 4:1 by volume)