反应详情

温度

100 °C

A mixture of 2-(3,4-difluoro-phenyl)-ethanol (5 g, 0.032 mol, from step (iii) above), 51.84 ml (49%, 0.64 mol) of HBr in acetic acid and 5 ml of sulfuric acid was stirred at 100° C. for 4 h. The reaction mixture was poured into ice and extracted with diethylether. Organic layer was washed with NaHCO3, water and dried over sodium sulfate. Solvent evaporation under reduced pressure followed by purification (three times) over silica gel using petroleum ether as eluent afforded (1.8 g) of the title compound as a liquid.

1. additionThe reaction mixture was poured into ice
2. extractionextracted with diethylether
3. washOrganic layer was washed with NaHCO3, water
4. dry with materialdried over sodium sulfate
5. customSolvent evaporation under reduced pressure
6. customfollowed by purification (three times) over silica gel