Reaktion #43322
ord-a7269e992a824e05b5d1f6a6b677604a
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeThe reaction liquid
- 2Temperaturwas cooled to room temperature
- 3Waschenwashed with water
- 4Trocknendried over anhydrous magnesium sulfate
- 5EinengenConcentrating the solvent under reduced pressure
- 6Sonstigethe 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%).