Reaktion #67278

Reaktionsgleichung

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

m-CPBA

m-CPBA

→

crude title compound

Ausbeute 189.4%

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

Ausbeute 189.4%

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux
2. 2
   Temperaturthe mixture was heated
3. 3
   Temperaturat reflux for another 22 h
4. 4
   Sonstigebrought to ambient temperature
5. 5
   FiltrationThe solid was filtered off
6. 6
   Waschenrinsed
7. 7
   WaschenThe resulting filtrate was washed with sodium bicarbonate (saturated), brine
8. 8
   Trocknenfurther dried (Na2SO4)
9. 9
   Sonstigeevaporated to dryness

Vorschrift

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).

Quelle