Reacción #43322

ord-a7269e992a824e05b5d1f6a6b677604a

Disolventes

Condiciones de reacción

Temperatura
80°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe reaction liquid
  2. 2
    Temperaturawas cooled to room temperature
  3. 3
    Lavadowashed with water
  4. 4
    Secadodried over anhydrous magnesium sulfate
  5. 5
    ConcentraciónConcentrating the solvent under reduced pressure
  6. 6
    Otrothe resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2)

Procedimiento

Potassium carbonate (2.4 g, 17.3 mmols) and sodium chlorodifluoroacetate (4.2 g, 27.5 mmols) were added to a DMF (20 mL) solution of 2-bromo-5-hydroxypyridine (2.4 g, 13.8 mmols) and stirred overnight at 80° C. The reaction liquid was cooled to room temperature, added ether, washed with water and dried over anhydrous magnesium sulfate. Concentrating the solvent under reduced pressure, the resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2) to provide the title compound (1.32 g, 43%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07732456B2uspto-grants-2010_06