反应详情

To a stirred solution of 3.0 ml of sodium bis(2-methoxyethoxy)aluminum hydride is added dropwise a solution of 2.2 g of 1-(p-chlorophenyl)-1,2-cyclopropanedicarboximide (U.S. Pat. No. 3,344,026) in 200 ml of benzene, over a 45 minute period, at room temperature, under nitrogen. The mixture is refluxed under nitrogen for one hour. After cooling, 4 ml of 5N sodium hydroxide is added to decompose any excess hydride and the mixture is diluted with 200 ml of water. The benzene phase is separated. The aqueous phase is extracted with ether. The ether and benzene phases are combined, dried over magnesium sulfate and concentrated under reduced pressure to give a white glass which is recrystallized from benzene-hexane to give the product as a white solid, mp 132°-137 ° C. (dec).

1. customat room temperature
2. temperatureThe mixture is refluxed under nitrogen for one hour
3. temperatureAfter cooling
4. customThe benzene phase is separated
5. extractionThe aqueous phase is extracted with ether
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customto give a white glass which
9. customis recrystallized from benzene-hexane