反应详情

温度

70 °C

3-Acetyl-7-chlorosulfonyl-8-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine (18 g, 0.056 m) was added in portions to a mixture of sodium sulfite (8.8 g, 0.069 m) and sodium bicarbonate (10.8 g, 0.115 m) in water (36 ml) stirred at 70° C. There was a vigorous evolution of gas after each addition. The mixture was stirred for fifteen minutes, treated with iodomethane (8.5 ml, 0.136 m) and refluxed for forty-five minutes. The mixture was partitioned between methylene chloride and water. The methylene chloride phase was washed with water, dried with sodium sulfate and concentrated in vacuo to give 3-acetyl-8-methoxy-7-methylsulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine, m.p. 159°-162° C.

1. additionafter each addition
2. stirringThe mixture was stirred for fifteen minutes
3. temperaturerefluxed for forty-five minutes
4. customThe mixture was partitioned between methylene chloride and water
5. washThe methylene chloride phase was washed with water
6. dry with materialdried with sodium sulfate
7. concentrationconcentrated in vacuo