Reacción #1485321

ord-ed8f84c6d80d48699fed7f146f08fbba

Condiciones de reacción

Temperatura
40°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGthe mixture was stirred at room temperature overnight
  2. 2
    Extracciónthe mixture was extracted with ethyl acetate
  3. 3
    LavadoThe extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
  4. 4
    Secadodried over anhydrous sodium sulfate
  5. 5
    OtroThe solvent was evaporated under reduced pressure

Procedimiento

Under an argon atmosphere, sodium ethoxide (20% ethanol solution, 1.7 g) was added to a mixture of diethyl (3,4-difluorophenyl)propanedioate (13.8 g) in tert-butylalcohol (50 mL) at room temperature, and the mixture was stirred at 40° C. for 30 min. Acrylonitrile (3.34 mL) was added to the reaction mixture at room temperature, and the mixture was stirred at room temperature overnight. Saturated aqueous ammonium chloride solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (15.2 g).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08901309B2uspto-grants-2014_12