反应详情

To a rapidly stirred solution of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-iodopyrazole (0.335 g) in toluene (2 ml) containing tetrakis(triphenylphosphine)palladium(0) (0.03 g) was added saturated aqueous sodium hydrogen carbonate solution (1 ml) and a solution of 2-fluorophenylboronic acid (0.210 g) in ethanol (1 ml). The mixture was heated under reflux for 5.5 hours, cooled and then poured into ether (25 ml) and water (25 ml). The organic layer was separated, washed with water (25 ml), brine (25 ml) and then dried (Na2SO4) and evaporated. The residue was purified by column chromatography on silica gel (40 g) eluted with dichloromethane. Combination and evaporation of suitable fractions gave the title compound as a white crystalline solid, m.p. 197° C.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 5.5 hours
3. temperaturecooled
4. customThe organic layer was separated
5. washwashed with water (25 ml), brine (25 ml)
6. dry with materialdried (Na2SO4)
7. customevaporated
8. customThe residue was purified by column chromatography on silica gel (40 g)
9. washeluted with dichloromethane
10. customCombination and evaporation of suitable fractions