反应详情

To a solution of ethyl 4-bromo-2-nitro-6-(trifluoromethyl)phenylcarbamate (275.3 mg) and potassium carbonate (108.3 mg) in N,N-dimethylformamide (5 ml) was added 3-trifluoromethylbenzyl bromide (0.180 ml). After the mixture was stirred at room temperature for 1 hour, 1N hydrochloric acid (ca. 30 ml) was added and the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, saturated brine, saturated aqueous sodium bicarbonate solution, and then saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The resultant residue was purified by silica gel column (35 g, hexane:ethyl acetate=20:1) to give the title compound (345.3 mg, 82%).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with 1N hydrochloric acid, saturated brine, saturated aqueous sodium bicarbonate solution
3. dry with materialsaturated brine, dried over anhydrous magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe resultant residue was purified by silica gel column (35 g, hexane:ethyl acetate=20:1)