반응 #168877

ord-831cdce3d3b94e2fbd5d876524cdd961

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under cooling on ice
  2. 2
    세척was then washed with a saturated sodium bicarbonate solution
  3. 3
    추출The water layer was extracted with chloroform
  4. 4
    건조The organic layer was dried over anhydrous sodium sulfate
  5. 5
    workup.DISTILLATIONthe solvent was then distilled away

실험 절차

The above 3-chloro-4-methoxy-2,5-dimethylpyridine 1-oxide (530 mg) was suspended in 15 ml of dichloromethane, and trifluoroacetic anhydride (0.39 ml) was then added to the suspension under cooling on ice. The resulting mixture was stirred at room temperature for 3 hours. The reaction solution was diluted with chloroform, and was then washed with a saturated sodium bicarbonate solution. The water layer was extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away, so as to obtain the title compound (521 mg) as an oily substance.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846703B2uspto-grants-2014_09