Reaktion #43322

ord-a7269e992a824e05b5d1f6a6b677604a

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction liquid
  2. 2
    Temperaturwas cooled to room temperature
  3. 3
    Waschenwashed with water
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    EinengenConcentrating the solvent under reduced pressure
  6. 6
    Sonstigethe resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2)

Vorschrift

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%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732456B2uspto-grants-2010_06