反应详情

A solution of N-trifluoroacetyl-8-chloro-7-methoxy-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (48 mg, 0.15 mmol) in dichloromethane (2 mL) was treated with BBr3 (0.30 mL of a 1.0M solution in CH2Cl2, 0.30 mmol) and stirred overnight at 20 C. The excess BBr3 was quenched with water and the resulting mixture diluted with ether (20 mL), washed with Na2CO3 (10 mL) and brine (10 mL), dried with Na2SO4 and concentrated. Flash chromatography (15% EtOAc in hexane, silica) resulted in 24 mg of a white solid. MS calculated for C13H13ClF3NO2+H: 308, observed: 308.

1. customThe excess BBr3 was quenched with water
2. additionthe resulting mixture diluted with ether (20 mL)
3. washwashed with Na2CO3 (10 mL) and brine (10 mL)
4. dry with materialdried with Na2SO4
5. concentrationconcentrated