Reacción #67303

ord-38de70a30356476493ede3110e26fb5d

Disolventes

Condiciones de reacción

Temperatura
50°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrobrought to ambient temperature
  2. 2
    FiltraciónThe solid was filtered off
  3. 3
    Lavadorinsed
  4. 4
    LavadoThe resulting filtrate was washed with sodium bicarbonate (saturated), brine
  5. 5
    Secadofurther dried (Na2SO4)
  6. 6
    Otroevaporated to dryness

Procedimiento

A solution of 1-[5-bromo-3-chloro-2-(oxiran-2-ylmethoxy)phenyl]ethanone (1.7 g, 5.6 mmol) and m-CPBA (2.4 g, 14 mmol) in DCM (30 ml) was heated to 50° C. After 22 h more m-CPBA (2.4 g, 14 mmol) was added and the mixture was heated at 50° C. for another 44 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 (2.7 g). MS m/z (rel. intensity, 70 eV) 280 (bp), 278 (84), 224 (54), 222 (52), 57 (79), 322 (M+, 5).

Fuente

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