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 (4 ml) at room temperature was added potassium carbonate (0.7 g), then allyl bromide (165 μl). The mixture was stirred at room temperature for 40 minutes. Water (50 ml) was then added, and the mixture was extracted with ether (50 ml, ×2). The combined organic layers were washed with water (50 ml), dried (Na2SO4), filtered 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 very pale yellow/white solid, m.p 115-116° C.

1. extractionthe mixture was extracted with ether (50 ml, ×2)
2. washThe combined organic layers were washed with water (50 ml)
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by column chromatography on silica gel (50 g)
7. washeluted with dichloromethane
8. customCombination and evaporation of suitable fractions