反应详情

To a stirred solution of 10 g of 4-chloro-2-nitrobenzyl alcohol in 200 mL of ether is added dropwise a solution of 17.7 g phosphorus tribromide in 100 mL of ether. The temperature of the reaction mixture is maintained at 15° or lower by means of cooling with an ice-water bath. On completion of the addition the reaction mixture is allowed to stir for an additional 1 hour at 15° and then at room temperature overnight. The reaction mixture is neutralized with 100 mL of 3N sodium hydroxide, and the layers are separated. The ethereal extracts are washed with 2×250 mL of brine, dried over anydrous sodium sulfate; the solvent is evaporated to dryness under reduced pressure to yield 4-chloro-2-nitrobenzyl bromide melting at 50°.

1. temperatureThe temperature of the reaction mixture is maintained at 15° or lower by means
2. temperatureof cooling with an ice-water bath
3. additionOn completion of the addition the reaction mixture
4. customat room temperature
5. customovernight
6. customthe layers are separated
7. washThe ethereal extracts are washed with 2×250 mL of brine
8. dry with materialdried over anydrous sodium sulfate
9. customthe solvent is evaporated to dryness under reduced pressure