Реакция #157995

ord-df3e9f22808e44b8a724cb76231ba676

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    КонцентрированиеThe reaction solution was concentrated under the reduced pressure
  2. 2
    workup.DISSOLUTIONthe resulting residues were dissolved in ethyl acetate
  3. 3
    ПромывкаThe solution was washed with water
  4. 4
    Сушкаdried over anhydrous magnesium sulfate
  5. 5
    ФильтрацияThe drying agent was filtered off
  6. 6
    Другоеthe solvent was removed by distillation under the reduced pressure
  7. 7
    ДругоеThe resulting residues were purified by column chromatography

Методика

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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08822691B2uspto-grants-2014_09