反应详情

62 ml of a 3 M methylmagnesium bromide solution in tetrahydrofuran is added in drops within one hour at 0 C. into 18.6 g of 5-bromo-2-methoxybenzoic acid methyl ester and 180 ml of diethyl ether. After 16 hours at room temperature and while being cooled with ice, it is mixed with saturated ammonium chloride solution and ethyl acetate. The ethyl acetate phase is washed with water, dried (Na2SO4) and concentrated by evaporation. After bulb tube distillation (boiling point: 140° C./0.04 hPa), 16.7 g of crystalline 1-(5-bromo-2-methoxyphenyl)-1-methylethanol is obtained. Flash point: 66-68° C.

1. temperaturewhile being cooled with ice, it
2. washThe ethyl acetate phase is washed with water
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated by evaporation
5. distillationAfter bulb tube distillation (boiling point: 140° C./0.04 hPa)