反应详情

温度

50 °C

To a solution of (±)-2-oxo-3-tert-butoxycarbonylamino-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (28.6 g) in N,N-dimethylformamide (50 mL), sodium hydrogencarbonate (17.3 g) and 3-bromocyclohexene (33.2 g) were added, followed by LZ stirring at 50° C. for 1 hour. The reaction mixture was allowed to cool down. Subsequent to addition of ice water, the reaction mixture was extracted with methylene chloride. The organic layer was washed with brine and then dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. Diisopropyl ether was added to the residue for crystallization. Crystals so precipitated were then collected by filtration. The crystals were washed with ethanol and then dried, whereby the title compound (30.1 g) was obtained. Yield: 82%.

1. temperatureto cool down
2. extractionthe reaction mixture was extracted with methylene chloride
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. additionDiisopropyl ether was added to the residue for crystallization
7. customCrystals so precipitated
8. filtrationwere then collected by filtration
9. washThe crystals were washed with ethanol
10. customdried