反应详情

To a solution of 4-[1-(3-bromo-4-methoxy-phenyl)-1-hydroxy-heptyl]-benzoic acid methyl ester (572 mg, 1.31 mmol) in dichloromethane (10 mL) is added TFA (749 mg, 6.57 mmol). 5 min later, triethylsilane (763 mg, 6.57 mmol) is added dropwise. 5 h later, the reaction mixture is diluted with ethyl acetate, washed with 1N NaOH, water, brine, dried over sodium sulfate, concentrated and purified by column chromatography to give 4-[1-(3-bromo-4-methoxy-phenyl)-hept-1-enyl]-benzoic acid methyl ester (380 mg), which is hydrolyzed by 5N NaOH (1 mL) to afford the titled compound (380 mg).

1. washwashed with 1N NaOH, water, brine
2. dry with materialdried over sodium sulfate
3. concentrationconcentrated
4. custompurified by column chromatography