反应详情

温度

23 °C

To a stirred suspension of 3-[7-(4-fluoro-phenyl)-4-oxo-4,5-dihydro-3H-benzo[b][1,4]diazepin-2-yl]-N-hydroxy-benzamidine (Example 167) (78 mg, 0.2 mmol) in EtOH (3 mL) was added at 23° C. sodium hydride (55% dispersion in oil, 32 mg, 0.8 mmol) and the mixture was stirred at 23° C. for 5 min. Butyrolactone (103 mg, 1.2 mmol) was added and the mixture was heated to 70° C. for 3 h. The reaction mixture was cooled to 23° C. and partitioned between ethyl acetate and H2O. The organic layer was dried over Na2SO4, evaporated in vacuum, and the residue was crystallized from dichloromethane to give the title compound as light yellow solid (60 mg).

1. temperaturethe mixture was heated to 70° C. for 3 h
2. temperatureThe reaction mixture was cooled to 23° C.
3. custompartitioned between ethyl acetate and H2O
4. dry with materialThe organic layer was dried over Na2SO4
5. customevaporated in vacuum
6. customthe residue was crystallized from dichloromethane