反应详情

A solution of 4-bromo-3-methylbenzaldehyde (4 g, 20 mmol) in dry tetrahydrofuran (40 mL) was cooled to 0° C. under nitrogen atmosphere, and then methyl magnesium bromide (20 mL, 1N in tetrahydrofuran) was added dropwise. The ice bath was removed, and the mixture was stirred for 2 hours. Ammonium chloride aqueous (40 mL) was added and the mixture was extracted with dichloromethane (20 mL*3). The organic phase was dried by sodium sulphate, filtered and concentrated to give a residue. The residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=5:1) to give 1-(4-bromo-3-methylphenyl)ethanol as a colorless oil (4.0 g, 93%).

1. customThe ice bath was removed
2. additionAmmonium chloride aqueous (40 mL) was added
3. extractionthe mixture was extracted with dichloromethane (20 mL*3)
4. dry with materialThe organic phase was dried by sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated
7. customto give a residue
8. customThe residue was purified by column chromatography (silica gel, petroleum ether/ethyl acetate=5:1)