反应详情

To a chloroform solution (8 mL) of [4-(benzyloxy)-5-bromo-2-chlorophenyl][4-[2-(methoxymethoxy)ethyl]phenyl]methanol (750 mg, 1.53 mmol) cooled in ice were added Et3SiH (367 μL, 2.30 mmol) and BF3.Et2O (232 μL, 1.83 mmol), and the mixture was stirred for an hour at the same temperature. To this solution cooled in ice was added a saturated sodium bicarbonate aqueous solution, and warmed to room temperature. The resulting mixture was extracted with ethyl acetate, washed with brine, and dried with anhydrous magnesium sulfate. The drying agent was filtered off, and the solvent was evaporated under reduced pressure. Thus obtained residue was purified with silica gel column chromatography (hexane:ethyl acetate=4:1) to obtain the title compound (290 mg, 40%) as a colorless oily compound.

1. temperatureTo this solution cooled in ice
2. extractionThe resulting mixture was extracted with ethyl acetate
3. washwashed with brine
4. dry with materialdried with anhydrous magnesium sulfate
5. filtrationThe drying agent was filtered off
6. customthe solvent was evaporated under reduced pressure
7. customThus obtained residue was purified with silica gel column chromatography (hexane:ethyl acetate=4:1)