反应详情

To a cooled and stirred solution of N-tert-butyl-3-{1-[6-(4-chloro-3-methyl-phenyl)-4-methyl-pyrimidin-2-yl]-1H-imidazol-4-yl}-benzenesulfonamide (0.53 g) in dichloromethane (5 ml) was added TFA (5 ml) and the reaction mixture was allowed to stir at room temperature for 15 h. The mixture was evaporated to dryness and saturated NaHCO3 solution (10 ml), diethylether and heptane were added. The mixture was stirred at room temperature for 1 h, the precipitate was collected by filtration, washed with water and heptane and dried. Further purification by flash chromatography on silica gel (ethyl acetate/heptane) and crystallization (THF/heptane) yielded the title compound as a white solid (0.3 g, 68%). MS (ISP) 440.1 [(M+H)+]; mp 219° C. (dec.).

1. temperatureTo a cooled
2. customThe mixture was evaporated to dryness and saturated NaHCO3 solution (10 ml), diethylether and heptane
3. additionwere added
4. stirringThe mixture was stirred at room temperature for 1 h
5. filtrationthe precipitate was collected by filtration
6. washwashed with water and heptane
7. customdried
8. customFurther purification by flash chromatography
9. customon silica gel (ethyl acetate/heptane) and crystallization (THF/heptane)