反应详情

To a suspension of 60% sodium hydride (143 mg) in N,N-dimethylformamide (3 ml) was added a solution of 5-bromo-3-methyl-1H-indazole (500 mg) in N,N-dimethylformamide (1 ml) at 0° C., and the mixture was stirred at the same temperature for 30 min. To the obtained reaction mixture was added (1-cyanocyclopropyl)methyl 4-methylbenzenesulfonate (420 mg), and the mixture was stirred at room temperature for 16 hr. To the reaction mixture was added saturated aqueous ammonium chloride solution, and the mixture was extracted with dichloromethane. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (60 mg).

1. customTo the obtained reaction mixture
2. stirringthe mixture was stirred at room temperature for 16 hr
3. extractionthe mixture was extracted with dichloromethane
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)