反应详情

温度

75 °C

To a stirred solution of sodium sulphite (1.60 g, 12.6 mmol) and sodium hydrogen carbonate (1.14 g, 13.56 mmol) in water (25 ml) was added 3-acetyl-7-chlorosulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine (2.6 g, 9.04 mmol) in tetrahydrofuran (10 ml). The reaction mixture was then heated at 75° C. for 2 h, cooled to 30° C. and methyl iodide (2.8 ml, 45.20 mmol) added. After stirring at 50° C. for 24 h, the reaction mixture was cooled to room temperature and partitioned between water (50 ml) and ethyl acetate (100 ml). The aqueous layer was then separated and further extracted with ethyl acetate (2×80 ml). The combined organics were then dried (Na2SO4) and the solvent removed in vacuo to give the title compound (1.77 g, 73%) as a pale yellow solid.

1. temperaturecooled to 30° C.
2. temperaturethe reaction mixture was cooled to room temperature
3. custompartitioned between water (50 ml) and ethyl acetate (100 ml)
4. customThe aqueous layer was then separated
5. extractionfurther extracted with ethyl acetate (2×80 ml)
6. dry with materialThe combined organics were then dried (Na2SO4)
7. customthe solvent removed in vacuo