反应详情

To a mixture of 10,11-dihydro-5H-pyrrolo [2,1-c][1,4] benzodiazepine (1.44 g) and triethylamine (0.95 g) in dichloromethane (40 mL) cooled in an ice bath, was added dropwise a solution of the crude 4-bromo-2-chlorobenzoyl chloride (2.42 g) in dichloromethane (20 mL). The cooling bath was removed and after stirring for 22 hours, the reaction mixture was sequentially washed with water, saturated aqueous sodium bicarbonate, 0.5 N hydrochloric acid and water. The dichloromethane solution was dried over anhydrous sodium sulfate, filtered and then evaporated to dryness to yield an off-white foam. Purification by flash chromatography on silica gel Merck-60 eluting with hexane-ethyl acetate (2:1) resulted in a white solid (3.02 g), m.p. 77-80° C.

1. temperaturecooled in an ice bath
2. customThe cooling bath was removed
3. washthe reaction mixture was sequentially washed with water, saturated aqueous sodium bicarbonate, 0.5 N hydrochloric acid and water
4. dry with materialThe dichloromethane solution was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. customevaporated to dryness
7. customto yield an off-white foam
8. customPurification by flash chromatography on silica gel
9. washeluting with hexane-ethyl acetate (2:1)