반응 #5251

ord-0d60770bcb50476997f7e87cec0a58de

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타evaporated
  2. 2
    농축The reaction mixture is concentrated under reduced pressure
  3. 3
    추출extracted with ethyl acetate
  4. 4
    세척The organic layer is washed with water
  5. 5
    기타dried
  6. 6
    기타evaporated
  7. 7
    기타The resulting crystalline residue is recrystallized from ethyl acetate

실험 절차

A mixture of 64.2 g of 1-ethoxycarbonyl-4-hydroxy-4-(3,4-dichlorophenyl)piperidine (X-1) and a solution of 72.4 g of KOH in 700 ml of nBuOH is refluxed for 2 hours and evaporated. The reaction mixture is concentrated under reduced pressure and extracted with ethyl acetate. The organic layer is washed with water, dried and evaporated. The resulting crystalline residue is recrystallized from ethyl acetate to prepare 44.7 g (Yield: 90.0%) of the compound (II-1). mp. 144.5°-146.0° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05243051uspto-grants-1993_09