反应详情

温度

130 °C

To a solution of (4-bromo-2-methanesulfonyl-phenyl)-methanol (preparation 112) (100 mg, 0.38 mmol) in POBr3 (542 mg, 1.89 mmol) was added PBr3 (511 mg, 1.89 mmol). After the addition, the reaction mixture was stirred at 130° C. overnight. TLC (petroleum ether:EtOAc 1:1) showed the reaction was complete. The reaction was cooled to room temperature and then poured into brine (10 mL) and extracted with EtOAc (10 mL×2). The combined organic layers were washed with brine (10 mL×2), dried over sodium sulfate and concentrated in vacuo to give crude 4-bromo-1-bromomethyl-2-methanesulfonyl-benzene (200 mg, 80%) as a white solid.

1. additionAfter the addition
2. temperatureThe reaction was cooled to room temperature
3. extractionextracted with EtOAc (10 mL×2)
4. washThe combined organic layers were washed with brine (10 mL×2)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo