반응 #591179

ord-a8d8f36575b6452ab537965589917248

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도by heating
  2. 2
    온도under reflux 1.5 hours
  3. 3
    농축The resulting mixture was concentrated under reduced pressure
  4. 4
    추출subjected to extraction with dichloromethane
  5. 5
    세척washed with water
  6. 6
    세척washed with a saturated sodium chloride solution
  7. 7
    건조dried over sodium sulfate
  8. 8
    여과filtrated
  9. 9
    농축concentrated under reduced pressure

실험 절차

Pyridinium p-toluenesulfonate (PPTS) (0.24 g) was added to a mixed solution of 5-(1,3-dioxolan-2-yl)-8-methoxy-1-(6-thiophen-3-ylpyridin-3-ylmethyl)-3,4-dihydro-1H-quinolin-2-one (0.4 g) in acetone (8 ml) and water (4 ml), followed by heating under reflux 1.5 hours. The resulting mixture was concentrated under reduced pressure, subjected to extraction with dichloromethane, washed with water, washed with a saturated sodium chloride solution, dried over sodium sulfate, filtrated, and concentrated under reduced pressure to thereby obtain 0.4 g (yield: quantitative) of 8-methoxy-1-(6-thiophen-3-ylpyridin-3-ylmethyl)-2-oxo-1,2,3,4-tetrahydroquinoline-5-carboxaldehyde as a light brown amorphous solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07777038B2uspto-grants-2010_08