Réaction #168876

ord-dbb251982fd84cea88e23d9109cbe504

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températureunder cooling on ice
  2. 2
    ExtractionThe water layer was extracted with chloroform two times
  3. 3
    SéchageThe organic layer was dried over anhydrous sodium sulfate
  4. 4
    workup.DISTILLATIONthe solvent was then distilled away

Mode opératoire

The above 3-chloro-4-methoxy-2,5-dimethylpyridine (181 mg) was dissolved in 5 ml of dichloromethane, and urea peroxide (169 mg) and phthalic anhydride (219 mg) were then added to the solution. The resulting mixture was stirred at room temperature for 2.5 hours. Thereafter, a saturated aqueous sodium thiosulfate solution was added to the reaction solution under cooling on ice, and the resulting mixture was then diluted with chloroform. The water layer was extracted with chloroform two times. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away, so as to obtain the title compound (181 mg) as a solid.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08846703B2uspto-grants-2014_09