تفاعل #5251

ord-0d60770bcb50476997f7e87cec0a58de

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىevaporated
  2. 2
    تركيزThe reaction mixture is concentrated under reduced pressure
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلThe organic layer is washed with water
  5. 5
    أخرىdried
  6. 6
    أخرىevaporated
  7. 7
    أخرىThe resulting crystalline residue is recrystallized from ethyl acetate

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05243051uspto-grants-1993_09