反应详情

A 16.60 g portion of 3-(p-chlorobenzoyl)-1-(p-chlorophenyl)-3-azabicyclo[3.1.0]hexane (prepared above) is dissolved in 160 ml of benzene and 55.5 g of sodium bis(2-methoxyethoxy)aluminum hydride (70% benzene solution) is added dropwise. The mixture is refluxed for 2 hours, cooled and quenched slowly with 10N sodium hydroxide. Water is added, the organic layer is separated and washed 3 times with water and then dried over sodium magnesium sulfate. Removal of the solvent yields an off-white solid, mp 88°-92° C.

1. temperatureThe mixture is refluxed for 2 hours
2. temperaturecooled
3. customquenched slowly with 10N sodium hydroxide
4. additionWater is added
5. customthe organic layer is separated
6. washwashed 3 times with water
7. dry with materialdried over sodium magnesium sulfate
8. customRemoval of the solvent
9. customyields an off-white solid, mp 88°-92° C.