反应详情

2-Oxo-3-tert-butoxycarbonylamino-5-(3-methyl-2-butenoyl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (1.54 g) was suspended in toluene (22 ml), 2-bromo-2′-methylacetophenone (1.05 g), 1N aqueous sodium hydroxide (11 ml) and tetra n-butylammonium bromide (25 mg) were added, and the mixture was stirred for 4 hours at room temperature. The reaction mixture was acidified with 1N hydrochloric acid, extracted with methylene chloride. The organic layer was washed with saturated aqueous sodium bicarbonate, dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography(chloroform:ethyl acetate=10:1), to thereby obtain 2.26 g of the titled compound (Yield: 100%).

1. extractionextracted with methylene chloride
2. washThe organic layer was washed with saturated aqueous sodium bicarbonate
3. dry with materialdried over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customthe residue was purified by silica gel column chromatography(chloroform:ethyl acetate=10:1)