反应详情

11 mg of sodium borohydride were added at 0° C. to a solution of 112 mg of 1-(diethylcarbamoyl)-3-(2-methyl-3-chlorophenylsulfonyl)-4-formylpyrazole [prepared as described in Example 9(3)] in 3.5 ml of methanol, and the resulting mixture was stirred for 30 minutes. At the end of this time, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride, 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 5:1 by volume mixture of hexane and ethyl acetate, to afford 114 mg (a quantitative yield) of the title compound as an oil.

1. extractionextracted with ethyl acetate
2. washThe extract was washed with a saturated aqueous solution of sodium chloride
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 5:1 by volume mixture of hexane and ethyl acetate