反应详情

To a solution of 4-bromo-2-chlorobenzyl alcohol (14.48 g) in N,N-dimethylformamide (72 ml) were added imidazole (5.34 g) and tert-butylchlorodiphenylsilane (19.8 g) under ice-cooling and the mixture was stirred for 1 hr. Water was added to the reaction mixture and the resulting product was extracted twice with hexane. The organic layers were combined, and washed successively with water, a saturated aqueous solution of sodium hydrogen-carbonate and saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated and the residue was subjected to silica gel column chromatography (hexane) to give the objective compound (29.22 g) as colorless oil.

1. temperaturecooling
2. extractionthe resulting product was extracted twice with hexane
3. washwashed successively with water
4. dry with materiala saturated aqueous solution of sodium hydrogen-carbonate and saturated brine and dried over anhydrous magnesium sulfate
5. customThe solvent was evaporated