反应详情

1,2,3,4-Tetrahydro-benzo[b]azepin-5-one from Example E5.5 (480 mg, 2.98 mmol) was dissolved in a mixture of dichloromethane (30 ml) and triethylamine (1.3 ml). Benzoyl chloride (0.46 g, 3.28 mmol) was added and the reaction mixture was heated for at reflux for 2 h. The mixture was cooled and reduced in vacuo. The residue was dissolved in EtOAc and washed with 1M KHSO4 (aq), water and brine. The organic layer was dried, filtered and reduced in vacuo. The residue was purified by flash chromatography on silica gel (eluant; 50% EtOAc: 50% hexane) to yield the title compound (440 mg, 56%).

1. temperaturethe reaction mixture was heated for
2. temperatureat reflux for 2 h
3. temperatureThe mixture was cooled
4. washwashed with 1M KHSO4 (aq), water and brine
5. customThe organic layer was dried
6. filtrationfiltered
7. customThe residue was purified by flash chromatography on silica gel (eluant; 50% EtOAc: 50% hexane)