Реакция #5251

Уравнение реакции

1-ethoxycarbonyl-4-hydroxy-4-(3,4-dichlorophenyl)piperidine

KOH

→

compound

Выход 90.0%

4-Hydroxy-4-(3,4-dichlorophenyl)piperidine

Выход 90.0%

Растворители

nBuOH

Условия реакции

Обработка

1. 1
   Другоеevaporated
2. 2
   КонцентрированиеThe reaction mixture is concentrated under reduced pressure
3. 3
   Экстракцияextracted with ethyl acetate
4. 4
   ПромывкаThe organic layer is washed with water
5. 5
   Другоеdried
6. 6
   Другоеevaporated
7. 7
   ДругоеThe resulting crystalline residue is recrystallized from ethyl acetate

Методика

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.

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