반응 #67278

반응 방정식

1-[5-bromo-3-fluoro-2-(oxiran-2-ylmethoxy)phenyl]ethanone

m-CPBA

m-CPBA

→

crude title compound

수율 189.4%

5-BROMO-3-FLUORO-2-(OXIRAN-2-YLMETHOXY)PHENYL ACETATE

수율 189.4%

용매

DCM

반응 조건

후처리

1. 1
   온도at reflux
2. 2
   온도the mixture was heated
3. 3
   온도at reflux for another 22 h
4. 4
   기타brought to ambient temperature
5. 5
   여과The solid was filtered off
6. 6
   세척rinsed
7. 7
   세척The resulting filtrate was washed with sodium bicarbonate (saturated), brine
8. 8
   건조further dried (Na2SO4)
9. 9
   기타evaporated to dryness

실험 절차

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).

출처