反应详情

2.71 g of sodium borohydride were added in small fractions over 35 minutes at 0° C. to a solution of 56.1 g of the raw product of Step A in 235 ml of methanol and the mixture was stirred for 25 minutes while allowing the temperature to rise to room temperature. The mixture was added to aqueous 1N hydrochloric acid solution and water was added with stirring. The decanted aqueous phase was extracted with methylene chloride and the organic phase was washed with water and evaporated to dryness under reduced pressure. The residue was chromatographed over silica gel and was eluted with methylene chloride to obtain 13.3 g of (R, S) 2,2,2-trifluoro-1-(m-phenoxy-phenyl)-ethanol.

1. customto rise to room temperature
2. additionwas added
3. stirringwith stirring
4. extractionThe decanted aqueous phase was extracted with methylene chloride
5. washthe organic phase was washed with water
6. customevaporated to dryness under reduced pressure
7. customThe residue was chromatographed over silica gel
8. washwas eluted with methylene chloride