反应详情

A solution of 3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-ethenylpyrazole (0.1 g), N-methylmorpholine oxide (0.005 g), osmium tetroxide (50 μl of a 2.5% solution in t-butanol) in water (5 ml) and acetone (45 ml) was stirred at room temperature for 16 hours. Sodium metaperiodate (0.005 g) was added and stirring continued for 16 hours. The reaction mixture was evaporated and the residue partitioned between ether and aqueous sodium hydrogen carbonate solution. The aqueous layer was separated and extracted with ether. The combined ether extracts were dried (Na2SO4) and evaporated. The residue was purified by column chromatography on silica gel (5 g) eluted with dichloromethane. Combination and evaporation of suitable fractions gave the title compound as a beige solid, m.p. 167.5-168.5° C.

1. customThe reaction mixture was evaporated
2. customthe residue partitioned between ether and aqueous sodium hydrogen carbonate solution
3. customThe aqueous layer was separated
4. extractionextracted with ether
5. dry with materialThe combined ether extracts were dried (Na2SO4)
6. customevaporated
7. customThe residue was purified by column chromatography on silica gel (5 g)
8. washeluted with dichloromethane
9. customCombination and evaporation of suitable fractions