Реакция #43322

ord-a7269e992a824e05b5d1f6a6b677604a

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe reaction liquid
  2. 2
    Температураwas cooled to room temperature
  3. 3
    Промывкаwashed with water
  4. 4
    Сушкаdried over anhydrous magnesium sulfate
  5. 5
    КонцентрированиеConcentrating the solvent under reduced pressure
  6. 6
    Другоеthe resulting residue was purified on silica gel column chromatography (C-300; hexane:ethyl acetate=100:1-100:2)

Методика

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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07732456B2uspto-grants-2010_06