反应详情

A solution of 3-acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine (2.3 g, 0.01 m) in acetic acid (20 ml) was treated with a solution of bromine (1.8 g, 0.011 m) in acetic acid (10 ml). The mixture was warmed to 70° for 1.5 hours, concentrated in vacuo and partitioned between water and ethyl acetate. The ethyl acetate phase was washed, dried with sodium sulfate and concentrated in vacuo to give 3-acetyl-8-bromo-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine. NMR (CDCl3) 6.7, 7.3; aryl protons.

1. temperatureThe mixture was warmed to 70° for 1.5 hours
2. concentrationconcentrated in vacuo
3. custompartitioned between water and ethyl acetate
4. washThe ethyl acetate phase was washed
5. dry with materialdried with sodium sulfate
6. concentrationconcentrated in vacuo