反应详情

Here, 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-[N-methyl-N-(6,7-dimethoxy-1,2,3,4-tetrahydronaphth-2-yl)-amino]-propane hydrochloride (1.4 g, 0.0027 mol) is added to a suspension of lithium aluminum hydride (0.24 g, 0.0062 mol) in diethyl ether (50 ml) and refluxed for 7 hours. Then water and 15% sodium hydroxide solution are added, the mixture is concentrated in vacuo and purified over silica gel (50 g) (32-63 μm) with methylene chloride and increasing amounts of ethanol (up to 15%) as eluant. Yield: 0.6 g. Mp: 92°-93° C.

1. temperaturerefluxed for 7 hours
2. concentrationthe mixture is concentrated in vacuo
3. custompurified over silica gel (50 g) (32-63 μm) with methylene chloride
4. temperatureincreasing amounts of ethanol (up to 15%) as eluant