反应详情

温度

40 °C

A solution of 4-phenylcyclohexanone (10 mmol, Lancaster) in benzene (5 ml) is added dropwise to a suspension of NaH (20 mmol) in absolute ethyl acetate (20 mmol) and the reaction mixture is stirred after complete evolution of the gas for 3 h at 40° C. Then it is mixed with water, the reaction mixture is extracted three times with ether, the combined organic phases are washed with water and saturated sodium chloride solution, dried over sodium sulphate and the solvent is removed in a vacuum. After column chromatography purification on silica gel with hexane/EtOAc 15:1 a clean product is obtained. tR 2.14; MS (pos. Ion.) m/z 217.26 [M+H]+. (J. Med. Chem. 1989, 32(2), 351-357).

1. extractionthe reaction mixture is extracted three times with ether
2. washthe combined organic phases are washed with water and saturated sodium chloride solution
3. dry with materialdried over sodium sulphate
4. customthe solvent is removed in a vacuum
5. customAfter column chromatography purification on silica gel with hexane/EtOAc 15:1 a clean product
6. customis obtained