反应详情

To a stirred solution of 3-[7-(1,3-dimethyl-1H-pyrazol-5-yl)-1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl]-1-butanol (0.25 g) (intermediate 9) in chloroform (8 ml), at room temperature, thionyl chloride (0.11 ml) was added dropwise. After 2h, saturated aqueous sodium hydrogencarbonate (5 ml) was added, the reaction mixture was extracted with dichloromethane (15 ml), the organic phase dried with sodium sulphate and the solvent evaporated under reduced pressure. The crude product was purified by chromatography on silica gel with 80% cyclohexane-ethyl acetate to give the title compound (0.23 g) as a white solid.

1. extractionthe reaction mixture was extracted with dichloromethane (15 ml)
2. dry with materialthe organic phase dried with sodium sulphate
3. customthe solvent evaporated under reduced pressure
4. customThe crude product was purified by chromatography on silica gel with 80% cyclohexane-ethyl acetate