反应详情

温度

50 °C

200 mg of 3-chloroperoxybenzoic acid were added to a solution of 150 mg of 4-cyano-1-(diethylcarbamoyl)-3-(2-ethyl-6-methylphenylthio)pyrazole [prepared as described in step (3) above] in 5 ml of 1,2-dichloroethane, and the resulting mixture was heated at 50° C. for 2 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, dried over anhydrous sodium sulfate and concentrated by evaporation under reduced pressure. The concentrate was purified by column chromatography through silica gel, eluted with a 6:1 by volume mixture of hexane and ethyl acetate, to afford 153 mg (yield 95%) of the title compound, melting at 101°-102° C.

1. extractionextracted with methylene chloride
2. washThe extract was washed with an aqueous solution of sodium hydrogencarbonate
3. dry with materialdried 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 a 6:1 by volume mixture of hexane and ethyl acetate