반응 #48493

ord-0f3d0ecf69574958ae540bf9fed29955

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture was concentrated under reduced pressure
  2. 2
    workup.ADDITIONdiluted with ethyl acetate
  3. 3
    기타The organic layer was separated
  4. 4
    건조dried over anhydrous sodium sulfate
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타The residue was purified by basic silica gel column chromatography (ethyl acetate to ethyl acetate/methanol 10/1)

실험 절차

After 3-((6-chloronaphthalen-2-yl)sulfonyl)propinoic acid (0.30 g), HOBt (0.23 g) and WSC (0.29 g) were dissolved in DMF (10 mL), 1-(piperidin-4-yl)-2-pyrrolidinone (0.17 g) and triethylamine (0.10 g) were added thereto, and the mixture was stirred at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, and diluted with ethyl acetate and an aqueous sodium bicarbonate solution. The organic layer was separated, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (ethyl acetate to ethyl acetate/methanol 10/1) to obtain the title compound (0.17 g, 39%) as a colorless powder.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745623B2uspto-grants-2010_06