Reaction #1876811

ord-e53b31a39b7e456887d2989addfbee81

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturethe reaction mixture was heated
  2. 2
    Otherto room temperature
  3. 3
    Extractionthe aqueous layer was extracted three times with diethyl ether
  4. 4
    Washwashed with an 1 M aqueous sodium hydroxide solution
  5. 5
    Dryingdried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Procedure

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).

Source

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