Реакция #157743

ord-dc5ef1fb50724008913e69dd4a136d44

Растворители

Условия реакции

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

Обработка

  1. 1
    ТемператураThe reaction solution was cooled to room temperature
  2. 2
    Экстракцияfollowed by extraction with ethyl acetate
  3. 3
    ПромывкаThe organic layer was washed with brine
  4. 4
    Сушкаdried over anhydrous magnesium sulfate
  5. 5
    Фильтрацияfiltered
  6. 6
    ДругоеThe solvent was then evaporated under reduced pressure
  7. 7
    ДругоеThe residue was purified by silica gel column chromatography (hexane only)

Методика

2,2,2-Trifluoroethyliodide (15.2 g) and potassium carbonate (10.0 g) were added to a solution of 4-bromo-2-chlorophenol (5.0 g) in N,N-dimethylformamide (20 mL), and the mixture was stirred at 80° C. for 20 hours. The reaction solution was cooled to room temperature and water was added, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane only) to give 4-bromo-2-chloro-1-(2,2,2-trifluoroethoxy)benzene as a colorless oil (3.0 g, 43%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08822503B2uspto-grants-2014_09