反应详情

To a solution of ethyl 3-[2-fluoro-4-[[5-(hydroxymethyl)-4-methoxy-2-thienyl]methoxy]phenyl]propanoate (1.6 g, 4.3 mmol) in anhydrous dichloromethane (10 mL), cooled to 0° C., is added Dess-Martin periodinane (2.76 g, 6.5 mmol). The reaction mixture is warmed to room temperature and stirred for 2 hours. The reaction mixture is diluted with water (15 mL), extracted with ethyl acetate, washed with water (15 mL), brine (15 mL), dried over sodium sulfate, filtered, and evaporated to dryness. The crude material is purified by silica gel chromatography eluting with hexane:ethyl acetate (8.8:1.2) to give the title compound (0.8 g, 50%). ESI/MS m/z 367.1 (M+H)+.

1. extractionextracted with ethyl acetate
2. washwashed with water (15 mL), brine (15 mL)
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. customevaporated to dryness
6. customThe crude material is purified by silica gel chromatography
7. washeluting with hexane:ethyl acetate (8.8:1.2)