反应详情

A mixed solution of sodium acetate (2.8 g), 3-bromo-4-(bromomethyl)-N-[(trimethysilyl)methyl]benzamide (6.5 g) in DMF (30 ml) was stirred for 3 hours at 70° C. The reaction liquor was returned to room temperature and diluted with t-butyl methyl ether. The mixture was washed with water and a saturated aqueous brine, subsequently dried over magnesium sulfate. After separating the drying agent by filtration, the reaction liquor was distilled off under reduced pressure, and the resulting mixture was purified by silica gel chromatography, to obtain 2-bromo-4-{[(trimethysilyl)methyl]carbamoyl}benzyl acetate (2.4 g).

1. customwas returned to room temperature
2. washThe mixture was washed with water
3. dry with materiala saturated aqueous brine, subsequently dried over magnesium sulfate
4. customAfter separating the drying agent
5. filtrationby filtration
6. distillationthe reaction liquor was distilled off under reduced pressure
7. customthe resulting mixture was purified by silica gel chromatography