反应详情

To a suspension of 6-bromo-2-methyl-4-[(phenylmethyl)oxy]-1H-benzimidazole (79.2 g, 250 mmol, STEP 1) in N,N-dimethylformamide (500 mL) was added sodium hydride (60% in mineral oil, 12.0 g, 300 mmol) at 0° C. After stirring at room temperature for 20 minutes, the reaction mixture was cooled to 0° C. To the mixture was added 4-methylbenzenesulfonyl chloride (47.6 g, 250 mmol) at 0° C., and the reaction mixture was stirred at room temperature for 30 minutes. The mixture was quenched with water (800 mL), and the white precipitates were collected by filtration, washed with diisopropyl ether (500 mL), and dried in vacuum at 70° C. for 7 hours to afford the title compound as a white solid (116 g, 98%).

1. temperaturethe reaction mixture was cooled to 0° C
2. stirringthe reaction mixture was stirred at room temperature for 30 minutes
3. customThe mixture was quenched with water (800 mL)
4. customthe white precipitates
5. filtrationwere collected by filtration
6. washwashed with diisopropyl ether (500 mL)
7. customdried in vacuum at 70° C. for 7 hours