Reacción #493552

ord-bd7553a183964d958459cf8281aae9d3

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Concentraciónconcentration under reduced pressure
  2. 2
    Otrogave an oil
  3. 3
    Lavadowashed with water (three times) and brine
  4. 4
    Secadodried over magnesium sulfate
  5. 5
    ConcentraciónConcentration under reduced pressure
  6. 6
    Otrogave a yellow oil
  7. 7
    Otropartitioned between diethyl ether and 5 N sodium hydroxide (15 mL)
  8. 8
    Extracciónextracted with methylene chloride twice

Procedimiento

tert-Butyl 4-cyano-2-(2-trifluoromethylphenyl)butanoate (7.2 g) was dissolved in methylene chloride (40 mL). Trifluoroacetic acid (50 mL) was added at 0° C. and the reaction was initiated. After stirring at room temperature for one hour, concentration under reduced pressure gave an oil. The resulting oil was dissolved in diethyl ether, washed with water (three times) and brine and dried over magnesium sulfate. Concentration under reduced pressure gave a yellow oil. The oil was dissolved again in diethyl ether and partitioned between diethyl ether and 5 N sodium hydroxide (15 mL). The resulting aqueous layer was made acidic with 5 N hydrochloric acid (16 mL) and extracted with methylene chloride twice to obtain the title compound (6.76 g) as a colorless transparent oil.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08754100B2uspto-grants-2014_06