反应详情

温度

50 °C

250 mg of 3-chloroperoxybenzoic acid were added to a solution of 179 mg of 1-(diethylcarbamoyl)-3-(3-chlorophenylthio)-4-difluoromethylpyrazole [prepared as described in step (4) above] in 4 ml of 1,2-dichloroethane, and the resulting mixture was heated at 50° C. for 1.5 hours. At the end of this time, the reaction mixture was poured into an aqueous solution of sodium sulfite and extracted with methylene chloride. The extract was washed with an aqueous solution of sodium hydrogencarbonate and with a saturated aqueous solution of sodium chloride, in that order, after which it was dried over anhydrous sodium sulfate and concentrated by evaporation under reduced pressure. The concentrate was purified by column chromatography through silica gel, eluted with an 8:1 by volume mixture of hexane and ethyl acetate, to afford 170 mg (yield 87%) of the title compound as an oil.

1. extractionextracted with methylene chloride
2. washThe extract was washed with an aqueous solution of sodium hydrogencarbonate and with a saturated aqueous solution of sodium chloride, in that order
3. dry with materialafter which it was dried over anhydrous sodium sulfate
4. concentrationconcentrated by evaporation under reduced pressure
5. customThe concentrate was purified by column chromatography through silica gel
6. washeluted with an 8:1 by volume mixture of hexane and ethyl acetate