反应详情

2-(3,5-Dimethoxyphenylthio)benzyl alcohol (7.9 g) was dissolved in methylene chloride (40 ml), then triphenylphosphine (11.2 g) and carbon tetrabromide (11.2 g) were added thereto, the mixture was stirred at room temperature for ten minutes, diluted with ethyl acetate, washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was evaporated in vacuo. The residue was purified by a silica gel column chromatography (developing solvent; hexane:ethyl acetate=3:1) to give 2-(3,5-dimethoxyphenylthio)-benzyl bromide (9.53 g, yield of 98%).

1. washwashed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution
2. dry with materialdried over anhydrous magnesium sulfate
3. customthe solvent was evaporated in vacuo
4. customThe residue was purified by a silica gel column chromatography (developing solvent; hexane:ethyl acetate=3:1)