反应详情

Under a nitrogen atmosphere, mix 9-bromo-6-hydroxy-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (6 g, 17.8 mmol), anhydrous pyridine (0.06 mL, 0.72 mmol), 4-(dimethylamino)pyridine (222 mg, 1.8 mmol) and acetic anhydride (30 mL). Heat the mixture at reflux for 8 h and stir at RT for another 8 h Concentrate, dilute the residue in EtOAc, wash with 1 N HCl, and then with saturated aqueous sodium bicarbonate solution. Dry (sodium sulfate) and concentrate to give the title compound that was used in the next step without further purification.

1. temperatureHeat the mixture
2. temperatureat reflux for 8 h
3. concentrationConcentrate
4. additiondilute the residue in EtOAc
5. washwash with 1 N HCl
6. dry with materialDry (sodium sulfate)
7. concentrationconcentrate