反应详情

A mixture of 1-acetyl-6-bromo-1H-indazole (Intermediate 65) (0.50 g) N-cyclopropyl-4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (Intermediate 5) (0.59 g) aqueous sodium carbonate (1M, 2.35 ml) and PdCl2dppf (0.237 g) in 1,2-dimethoxyethane (30 ml) was stirred at reflux under nitrogen for 16 h. More sodium carbonate (2.3 ml) and catalyst (120 mg) were added and reflux was continued for a further 4 h. Conc. hydrochloric acid (1 ml) was added and the mixture was heated for a further 1 h. The mixture was absorbed onto silica then purified by column chromatography on silica eluting with cyclohexane:ethyl acetate (2:1 to 1:4) to give the title compound (0.25 g).

1. temperatureat reflux under nitrogen for 16 h
2. temperaturereflux
3. temperaturethe mixture was heated for a further 1 h
4. customThe mixture was absorbed onto silica
5. customthen purified by column chromatography on silica eluting with cyclohexane:ethyl acetate (2:1 to 1:4)