반응 #157791

ord-d520d21861fa4623b53270a7bb516f6f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출followed by extraction with ethyl acetate
  2. 2
    세척The organic layer was washed with brine
  3. 3
    건조dried over sodium sulfate
  4. 4
    여과After filtration
  5. 5
    기타the solvent was evaporated under reduced pressure
  6. 6
    기타the residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1→0:1)
  7. 7
    여과This was powdered with ethyl acetate, and filtration operation

실험 절차

Acetic anhydride (5 mL) was added to 6-[(E)-1-(4-aminophenyl)-2-cyclopentylethenyl]-3-chloropyridin-2(1H)-one (173 mg), and the mixture was stirred at room temperature for 15 minutes. Saturated aqueous sodium bicarbonate was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with brine and dried over sodium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1→0:1). This was powdered with ethyl acetate, and filtration operation gave the title compound as a light yellow powder (75 mg, 38%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822503B2uspto-grants-2014_09