反应详情

温度

50 °C

366 mg of 3-chloroperoxybenzoic acid were added to a solution of 245 mg of 1-(diethylcarbamoyl)-3-(2-ethyl-6methylphenylthio)pyrazole [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 hour. At the end of this time, the reaction mixture was mixed with an aqueous solution of sodium sulfite, after which it was extracted with methylene chloride. The extract was washed with an aqueous solution of sodium hydrogencarbonate and dried over anhydrous sodium sulfate, and then the solvent was removed by distillation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, eluted with an 8:1 by volume mixture of hexane and ethyl acetate, to give 266 mg (yield 99%) of the title compound as an oil.

1. extractionafter which it was extracted with methylene chloride
2. washThe extract was washed with an aqueous solution of sodium hydrogencarbonate
3. dry with materialdried over anhydrous sodium sulfate
4. customthe solvent was removed by distillation under reduced pressure
5. customThe resulting residue was purified by column chromatography through silica gel
6. washeluted with an 8:1 by volume mixture of hexane and ethyl acetate