Reaktion #1876811

ord-e53b31a39b7e456887d2989addfbee81

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture was heated
  2. 2
    Sonstigeto room temperature
  3. 3
    Extraktionthe aqueous layer was extracted three times with diethyl ether
  4. 4
    Waschenwashed with an 1 M aqueous sodium hydroxide solution
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Vorschrift

Potassium carbonate (22.6 g) and then a mixture of methyl ethyl ketone (MEK) (150 mL) and ethyl iodide (47.8 g) were added to a mixture of MEK (310 mL) and 3-trifluoromethylphenol (a) (25.0 g) at room temperature, and the reaction mixture was heated and stirred for 2 hours. After returning the mixture to room temperature, water was added for liquid separation and the aqueous layer was extracted three times with diethyl ether. The organic layers were combined, washed with an 1 M aqueous sodium hydroxide solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 19.3 g of Compound (b).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07070838B2uspto-grants-2006_07