Reaktion #157743

ord-dc5ef1fb50724008913e69dd4a136d44

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    TemperaturThe reaction solution was cooled to room temperature
  2. 2
    Extraktionfollowed by extraction with ethyl acetate
  3. 3
    WaschenThe organic layer was washed with brine
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    SonstigeThe solvent was then evaporated under reduced pressure
  7. 7
    SonstigeThe residue was purified by silica gel column chromatography (hexane only)

Vorschrift

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%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822503B2uspto-grants-2014_09