Reacción #67278
ord-dbc3b18dcb914fe7bf3e099e362727d2
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Temperaturaat reflux
- 2Temperaturathe mixture was heated
- 3Temperaturaat reflux for another 22 h
- 4Otrobrought to ambient temperature
- 5FiltraciónThe solid was filtered off
- 6Lavadorinsed
- 7LavadoThe resulting filtrate was washed with sodium bicarbonate (saturated), brine
- 8Secadofurther dried (Na2SO4)
- 9Otroevaporated to dryness
Procedimiento
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).