HRID28141

反应详情

EQUATION

反应方程式

HRID 28141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred and warm (40° C.) solution of 12 parts of potassium hydroxide in 200 parts of 2-propanol are added at once 21 parts of ethyl 4-{N-(4-chlorophenyl)-N-[(3-methoxyphenyl)acetyl]-amino}-1-piperidinecarboxylate and the whole is stirred and refluxed for 17 hours. The reaction mixture is cooled, filtered and evaporated. The semi-solid residue is acidified with a diluted hydrochloric acid solution, washed with 1,1'-oxybisethane and the aqueous acid phase is alkalized with sodium hydroxide solution. The free base is extracted with trichloromethane. The extract is dried and evaporated. The residue is crystallized from a mixture of 1,1'-oxybisethane and hexane, yielding 7.8 parts of N-(4-chlorophenyl)-3-methoxy-N-(4-piperidinyl)benzeneacetamide; mp. 85.7° C.

WORKUP

后处理

  1. stirringthe whole is stirred
  2. temperaturerefluxed for 17 hours
  3. temperatureThe reaction mixture is cooled
  4. filtrationfiltered
  5. customevaporated
  6. washwashed with 1,1'-oxybisethane
  7. extractionThe free base is extracted with trichloromethane
  8. customThe extract is dried
  9. customevaporated
  10. customThe residue is crystallized from a mixture of 1,1'-oxybisethane and hexane