反应详情

温度

-5 °C

260 g (crude product of several batches, about 1.05 mol) of (3-bromo-4-chlorophenyl)methanol were dissolved in 2.86 liters of dichloromethane, the mixture was cooled to −5° C. and 127.1 g (44.6 ml, 459.6 mmol) of phosphorus tribromide were added slowly. After the addition had ended, the mixture was stirred at −5° C. for another 1 h and then diluted with dichloromethane and water. The organic phase was separated off, dried over magnesium sulphate and concentrated under reduced pressure. This gave, as a crude product, 280.5 g (about 84% of theory) of 2-bromo-4-(bromomethyl)-1-chlorobenzene.

1. additionAfter the addition
2. customThe organic phase was separated off
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated under reduced pressure