반응 #55037

ord-808cb0a0266748a798ce898cc0ed978c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 47 hours
  2. 2
    workup.STIRRINGstirring
  3. 3
    온도refluxing
  4. 4
    온도The reaction mixture is cooled
  5. 5
    여과filtered
  6. 6
    세척The filtrate is washed with water
  7. 7
    기타dried
  8. 8
    기타evaporated in vacuo
  9. 9
    여과The precipitated solid salt is filtered off
  10. 10
    기타dried

실험 절차

To a stirred solution of 4 parts of N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide and 3 parts of N,N-dimethylethanamine in 200 parts of benzene are added portionwise 4 parts of 1-iodopropane and the whole is stirred and refluxed for 47 hours. Then the second portion of 4 parts of 1-iodopropane is added and stirring and refluxing is continued for another 20h.20. The reaction mixture is cooled and filtered. The filtrate is washed with water, dried and evaporated in vacuo. From the oily free base, the hydrochloride salt is prepared in the conventional manner in 1,1'-oxybisethane. The precipitated solid salt is filtered off and dried, yielding 3.5 parts of N-(4-chlorophenyl)-N-(1-propyl-4-piperidinyl)benzeneacetamide hydrochloride; mp. 235.5° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04151286uspto-grants-1979_04