反应详情

温度

60 °C

A mixture of 1-(5-bromo-3-fluoro-2-hydroxyphenyl)ethanone (3.7 g, 15.8 mmol), epibromohydrin (2.6 ml, 31.7 mmol) and K2CO3 (3.3 g, 23.8 mmol) in DMF (20 ml) was heated at 60° C. for 1 h 50 min. The solution was brought to ambient temperature and water and EtOAc was added. The water phase was extracted with EtOAc. The combined organic phases were washed with LiCl (5%), HCl (1 N) and brine and were dried (Na2SO4) and evaporated to dryness. Purification on flash column chromatography (isooctane/EtOAc) gave the title compound (3.9 g). MS m/z (rel. intensity, 70 eV) 289 (M+, 13), 288 (M+, 14), 218 (91), 217 (bp), 81 (39), 57 (95).

1. customwas brought to ambient temperature
2. extractionThe water phase was extracted with EtOAc
3. washThe combined organic phases were washed with LiCl (5%), HCl (1 N) and brine
4. dry with materialwere dried (Na2SO4)
5. customevaporated to dryness
6. customPurification on flash column chromatography (isooctane/EtOAc)