反应 #5251

ord-0d60770bcb50476997f7e87cec0a58de

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他evaporated
  2. 2
    浓缩The reaction mixture is concentrated under reduced pressure
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤The organic layer is washed with water
  5. 5
    其他dried
  6. 6
    其他evaporated
  7. 7
    其他The resulting crystalline residue is recrystallized from ethyl acetate

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05243051uspto-grants-1993_09