反应详情

温度

-40 °C

Under a nitrogen atmosphere, 1,1-dichloroethane (30.0 g, 303 mmol), diphenylethylene (5.59 g, 31.0 mmol) and diethyl ether (62 ml) were placed in a reaction flask and cooled to −40° C. To the mixture, n-butyllithium in hexane (45 ml, 1.56M, 70.2 mmol) was added gradually and the mixture was stirred at the same temperature for one hour, followed by warming to room temperature. Then, water was added to the reaction mixture and the organic layer was extracted with toluene. The toluene extract was dried over anhydrous magnesium sulfate and then the solvent was removed under reduced pressure. The concentrate was recrystallized from ethanol to give the title compound (5.91 g, 78%) as white crystal.

1. temperatureby warming to room temperature
2. extractionthe organic layer was extracted with toluene
3. extractionThe toluene extract
4. dry with materialwas dried over anhydrous magnesium sulfate
5. customthe solvent was removed under reduced pressure
6. customThe concentrate was recrystallized from ethanol