反应详情

温度

0 °C

To a solution of lithium aluminum hydride (2.53 g) in diethyl ether (50 mL) was added aluminum chloride (2.96 g), and the mixture was stirred at 0° C. for 30 min. To the reaction mixture was added dropwise a solution of (3RS)-3-(3,4-dichlorophenyl)-3-hydroxy-4-(4-methoxyphenoxy)butanenitrile (11.7 g) in THF (50 mL), and the mixture was stirred at 0° C. for 15 min, and then stirred while warming to room temperature for 2 hr. To the reaction mixture was added ice, and the precipitate was filtered off through celite. The filtrate was diluted with water, and the mixture was extracted with ethyl acetate. The obtained extract was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give the title compound (10.8 g).

1. stirringthe mixture was stirred at 0° C. for 15 min
2. stirringstirred
3. temperaturewhile warming to room temperature for 2 hr
4. additionTo the reaction mixture was added ice
5. filtrationthe precipitate was filtered off through celite
6. additionThe filtrate was diluted with water
7. extractionthe mixture was extracted with ethyl acetate
8. extractionThe obtained extract
9. washwas washed with brine
10. dry with materialdried over anhydrous magnesium sulfate
11. customThe solvent was evaporated under reduced pressure