反应详情

To a solution of 2-ethoxy-4′-fluoro-biphenyl-4-carboxylic acid ethyl ester (0.50 g, 1.73 mmol, 1.0 equiv) in anhydrous THF (10 mL) was added slowly over a time period of 15 min under cooling to −10° C. a solution of diisobutylaluminium hydride (5.2 mL, 5.20 mmol, 3.0 equiv; 1 M solution in hexane). After 1 h, the reaction mixture was poured on ice, the pH adjusted to 4 by addition of a 1 M solution of HCl, the solution extracted with ethyl acetate (2×100 mL) and the combined organic phases washed with water (2×100 mL) and a conc. solution of sodium chloride (100 mL). The organic phase was dried over MgSO4, concentrated by evaporation under reduced pressure to give 0.42 g (99%) of the title compound which was directly used in the consecutive step without further purification.

1. additionthe reaction mixture was poured on ice
2. extractionthe solution extracted with ethyl acetate (2×100 mL)
3. washthe combined organic phases washed with water (2×100 mL)
4. dry with materialThe organic phase was dried over MgSO4
5. concentrationconcentrated by evaporation under reduced pressure