反应详情

A solution of 1-[5-bromo-3-fluoro-2-(oxiran-2-ylmethoxy)phenyl]ethanone (1.3 g, 4.5 mmol) and m-CPBA (4.0 g, 18 mmol) in DCM (25 ml) was heated at reflux. After 22 h more m-CPBA (2.7 g, 12 mmol) was added and the mixture was heated at reflux for another 22 h and then brought to ambient temperature. The solid was filtered off and rinsed. The resulting filtrate was washed with sodium bicarbonate (saturated), brine and further dried (Na2SO4) and evaporated to dryness to give the crude title compound (2.6 g). MS m/z (rel. intensity, 70 eV) 305 (M+, 5), 304 (M+, 6), 263 (97), 262 (bp), 206 (49), 57 (65).

1. temperatureat reflux
2. temperaturethe mixture was heated
3. temperatureat reflux for another 22 h
4. custombrought to ambient temperature
5. filtrationThe solid was filtered off
6. washrinsed
7. washThe resulting filtrate was washed with sodium bicarbonate (saturated), brine
8. dry with materialfurther dried (Na2SO4)
9. customevaporated to dryness