反应详情

温度

0 °C

2-[3,4-Bis(difluoromethoxy)phenyl]ethanol (6 g, 0.024 mol; see step (iv) above) and triphenylphosphine (12.6 g, 0.048 mol) were taken up in dichloromethane (100 mL) and cooled to 0° C. CBr4 (15.9 g, 0.048 mol) in dichloromethane was added dropwise, and the mixture stirred at RT overnight under a nitrogen atmosphere. The reaction mixture was filtered, the filtrate concentrated under reduced pressure and the residue purified by column chromatography over silica gel (using 20% ethyl acetate in petroleum ether as eluent) to give the title compound as a yellow liquid. Yield 5.2 g.

1. filtrationThe reaction mixture was filtered
2. concentrationthe filtrate concentrated under reduced pressure
3. customthe residue purified by column chromatography over silica gel (using 20% ethyl acetate in petroleum ether as eluent)