Réaction #43322

ord-a7269e992a824e05b5d1f6a6b677604a

Solvants

Conditions de réaction

Température
80°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreThe reaction liquid
  2. 2
    Températurewas cooled to room temperature
  3. 3
    Lavagewashed with water
  4. 4
    Séchagedried over anhydrous magnesium sulfate
  5. 5
    ConcentrationConcentrating the solvent under reduced pressure
  6. 6
    Autrethe resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2)

Mode opératoire

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%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07732456B2uspto-grants-2010_06