Reacción #44697

ord-63c7feb226134404a5bf0269df3955a5

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe mixture is heated
  2. 2
    Temperaturaat reflux for 45 min
  3. 3
    FiltraciónThe mixture is filtered
  4. 4
    Lavadothe filtercake is washed with ethyl acetate and DCM
  5. 5
    OtroThe solvent is removed under reduced pressure

Procedimiento

1.00 g (7.19 mmol) of 2,6-difluorobenzonitrile is initially charged in 10 ml of acetonitrile. 1.99 g (14.4 mmol) of potassium carbonate and 1.03 g (7.19 mmol) of 3-chloro-4-hydroxyaniline are added, and the mixture is heated at reflux for 45 min. The mixture is filtered and the filtercake is washed with ethyl acetate and DCM. The solvent is removed under reduced pressure and the residue is by column chromatography (silica gel 60, gradient column: mobile phase: DCM:petroleum ether=2:1, then DCM).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07737153B2uspto-grants-2010_06