反应详情

温度

-20 °C

To 125 ml. of a 0.8 molar ethereal ethyl lithium solution a solution of 12.25 g. of 4-fluoro-4'-benzyloxy-benzophenone in 180 ml. of dry ether is added dropwise, in argon atmosphere, with stirring at -20° C. The reaction mixture is allowed to warm up to room temperature and stirred for further 90 minutes. It is then poured into saturated aqueous ammonium chloride solution under cooling. The aqueous phase is extracted with ether, the organic phases are combined and washed to neutral with water. After drying over anhydrous magnesium sulfate ether is distilled off under reduced pressure. The solid residue is crystallized from a mixture of ethyl acetate and n-heptane to yield 7.4 g. of the named compound, melting at 56°-57° C.

1. temperatureto warm up to room temperature
2. stirringstirred for further 90 minutes
3. temperatureunder cooling
4. extractionThe aqueous phase is extracted with ether
5. washwashed to neutral with water
6. dry with materialAfter drying over anhydrous magnesium sulfate ether
7. distillationis distilled off under reduced pressure
8. customThe solid residue is crystallized from a mixture of ethyl acetate and n-heptane
9. customto yield 7.4 g