反应详情

To a stirred solution of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoroacetylpyrazole (1 g) in anhydrous N,N-dimethylformamide (5 ml) at room temperature was added potassium carbonate (0.69 g), then iodomethane (97 μl). The mixture was stirred at room temperature for one hour. Water (30 ml) was then added, and the mixture was extracted with ether (50 ml, ×2). The combined organic layers were washed with water (30 ml, ×2), and evaporated. The residue was purified by column chromatography on silica gel (50 g) eluted with dichloromethane. Combination and evaporation of suitable fractions gave the title compound as a white solid, m.p 160-161° C.

1. extractionthe mixture was extracted with ether (50 ml, ×2)
2. washThe combined organic layers were washed with water (30 ml, ×2)
3. customevaporated
4. customThe residue was purified by column chromatography on silica gel (50 g)
5. washeluted with dichloromethane
6. customCombination and evaporation of suitable fractions