Reacción #67278

ord-dbc3b18dcb914fe7bf3e099e362727d2

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaat reflux
  2. 2
    Temperaturathe mixture was heated
  3. 3
    Temperaturaat reflux for another 22 h
  4. 4
    Otrobrought to ambient temperature
  5. 5
    FiltraciónThe solid was filtered off
  6. 6
    Lavadorinsed
  7. 7
    LavadoThe resulting filtrate was washed with sodium bicarbonate (saturated), brine
  8. 8
    Secadofurther dried (Na2SO4)
  9. 9
    Otroevaporated 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).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08524766B2uspto-grants-2013_09