反应详情

温度

80 °C

Sodium bicarbonate (606 mg) and 3-bromocyclooctene (1.36 g) were added to a solution of 2-oxo-3-tert-butoxycarbonylamino-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (1 g) in N,N-dimethylformamide (20 ml), the mixture was stirred overnight at 80° C. After the reaction mixture was allowed to cool, ice-water was added thereto, extracted with ethyl acetate, the organic layer was washed with saturated brine. The resultant mixture was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and diisopropyl ether was added to the residue for crystallization, and collected by filtration, to thereby obtain 615 mg of the title compound as the mixture of diastereomer compounds.

1. temperatureto cool
2. extractionextracted with ethyl acetate
3. washthe organic layer was washed with saturated brine
4. dry with materialThe resultant mixture was dried over anhydrous sodium sulfate
5. customthe solvent was evaporated under reduced pressure, and diisopropyl ether
6. additionwas added to the residue for crystallization
7. filtrationcollected by filtration