HRID26758

反应详情

EQUATION

反应方程式

HRID 26758 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 refluxing mixture of 5 parts of 4-chloro-N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide, 5 parts of sodium carbonate, 0.4 parts of potassium iodide and 200 parts of butanol is added 4.7 parts of 1-iodopropane and the whole is stirred and refluxed for 22 hours. Then a second portion of 4.5 parts of 1-iodopropane is added and stirring and refluxing is continued for 27h.30. The reaction mixture is cooled, filtered and the filtrate is evaporated. The semi-solid residue is dissolved in methylbenzene. The solution is filtered from some impurities and the filtrate is evaporated again. The residue is crystallized from 1,1'-oxybisethane at -10° C.; yielding 0.9 parts of 4-chloro-N-(4-chlorophenyl)-N-(1-propyl-4-piperidinyl)benzeneacetamide; mp. 118.6° C.

WORKUP

后处理

  1. temperaturerefluxing
  2. stirringthe whole is stirred
  3. temperaturerefluxed for 22 hours
  4. stirringstirring
  5. temperaturerefluxing
  6. temperatureThe reaction mixture is cooled
  7. filtrationfiltered
  8. customthe filtrate is evaporated
  9. dissolutionThe semi-solid residue is dissolved in methylbenzene
  10. filtrationThe solution is filtered from some impurities
  11. customthe filtrate is evaporated again
  12. customThe residue is crystallized from 1,1'-oxybisethane at -10° C.