Reacción #157995

ord-df3e9f22808e44b8a724cb76231ba676

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    ConcentraciónThe reaction solution was concentrated under the reduced pressure
  2. 2
    workup.DISSOLUTIONthe resulting residues were dissolved in ethyl acetate
  3. 3
    LavadoThe solution was washed with water
  4. 4
    Secadodried over anhydrous magnesium sulfate
  5. 5
    FiltraciónThe drying agent was filtered off
  6. 6
    Otrothe solvent was removed by distillation under the reduced pressure
  7. 7
    OtroThe resulting residues were purified by column chromatography

Procedimiento

2-Cyano-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]quinoline-6-carboxamide (240 mg) was dissolved in dichloromethane, added with urea-hydrogen peroxide adduct (85 mg) and trifluoroacetic anhydride (190 mg), and stirred at room temperature for 20 hours. The reaction solution was concentrated under the reduced pressure, and the resulting residues were dissolved in ethyl acetate. The solution was washed with water and dried over anhydrous magnesium sulfate. The drying agent was filtered off and the solvent was removed by distillation under the reduced pressure. The resulting residues were purified by column chromatography to obtain 2-cyano-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]quinoline-6-carboxamide-1-oxide (0.20 g, 81%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08822691B2uspto-grants-2014_09