反应详情

To dichloromethane solution (30 ml) of 4-(4-t-butyldimethylsilyloxyphenyl)-4-hydroxy-7-methoxymethyloxy-3-[4-(methoxymethyloxy)phenyl]-3-methylthiochroman (1.134 g, 1.95 mmol) were added zinc iodide (1.367 g, 4.9 mmol) and sodium cyanoborohydride (797 mg, 12.7 mmol), and the resulting mixture was stirred for 2 hours at room temperature. After adding acetone (5 ml) and water, the reaction solution was extracted with dichloromethane and the organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the organic solvent. The crude product thus obtained was purified with silica gel column chromatography (ethyl acetate:hexane=1:4) to obtain 783 mg (yield: 71%) of the title compound.

1. extractionthe reaction solution was extracted with dichloromethane
2. washthe organic layer was washed with saturated saline
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationdistilled under reduced pressure
5. customto remove the organic solvent
6. customThe crude product thus obtained
7. customwas purified with silica gel column chromatography (ethyl acetate:hexane=1:4)