반응 #314448

ord-5d424983c19e4484a8c8c5c927e205be

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture was heated
  2. 2
    온도to reflux for 5 h
  3. 3
    기타Potassium chloride precipitated
  4. 4
    여과it was filtered off
  5. 5
    농축The liquid phase was concentrated until only one third of the liquid
  6. 6
    기타The solid formed during the concentration of the liquid phase
  7. 7
    여과was filtered
  8. 8
    세척washed thoroughly with ethanol

실험 절차

30 g (0.26 mol) of indole were dissolved in a solution of potassium hydroxide (77.6 g, 1.38 mol) in methanol (692 ml). 4-piperidone monohydrate hydrochloride (102.3 g, 0.66 mol) was added in one portion and the mixture was heated to reflux for 5 h. Potassium chloride precipitated upon cooling at room temperature and it was filtered off. The liquid phase was concentrated until only one third of the liquid remained in the round-bottom flask. The solid formed during the concentration of the liquid phase was filtered and washed thoroughly with ethanol and, finally, with ethyl ether. 31.9 g (63% of yield) of the final product were obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07560471B2uspto-grants-2009_07