反应详情

2-Oxo-3-tert-butoxycarbonylamino-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (1.0 g) was suspended in 1,2-dichloroethane (20 ml), and 2,2-dimethylbutanoyl chloride (538 mg) and pyridine (0.33 ml) were added thereto to the suspension, and the mixture was refluxed for 2 hours. Methylene chloride was added to the reaction mixture, washed with water and saturated aqueous sodium bicarbonate, dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, crystals so precipitate were washed with ether, to thereby obtain 1.20 g of the title compound (Yield 89.8%).

1. temperatureto the suspension, and the mixture was refluxed for 2 hours
2. washwashed with water and saturated aqueous sodium bicarbonate
3. dry with materialdried over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure, crystals so precipitate
5. washwere washed with ether