反应详情

温度

0 °C

A solution of AD-mix-α (66.0 g), t-BuOH (340 mL), and H2O (380 mL) was stirred until no solid was observed and then cooled to 0° C. Ethyl 3-(3-ethenyl-4,5-difluorophenyl)propanoate (16.3 g, 68.0 mmol) in t-BuOH (45 mL) and H2O (5 mL) was added and the reaction stirred at 0° C. for 6 h and then warmed to room temperature overnight. Sodium sulfite (84 g) was added and the reaction stirred at room temperature for 5 h. The reaction was diluted with H2O and extracted two times with CH2Cl2. The combined organic layers were dried over Na2SO4, filtered, and concentrated. Column chromatography (2-90% ethyl acetate:hexane) afforded the desired product (17.76 g, 95%).

1. temperaturewarmed to room temperature overnight
2. stirringthe reaction stirred at room temperature for 5 h
3. extractionextracted two times with CH2Cl2
4. dry with materialThe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated