반응 #55033

ord-0fb7ca53bca64e0fa512792348c1f012

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도warm
  2. 2
    workup.STIRRINGthe whole is stirred
  3. 3
    온도refluxed for 21h.30
  4. 4
    workup.STIRRINGstirring
  5. 5
    온도at reflux temperature
  6. 6
    온도The reaction mixture is cooled
  7. 7
    여과filtered
  8. 8
    기타the filtrate is evaporated
  9. 9
    기타on triturating in 1,1'-oxybisethane
  10. 10
    여과The solid product is filtered off
  11. 11
    기타crystallized from 1,1'-oxybisethane

실험 절차

to a stirred and warm (40° C.) mixture of 5 parts of N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide, 5 parts of sodium carbonate, a few crystals of potassium iodide and 200 parts of nbutanol is added 3.75 parts of bromocyclopentane and the whole is stirred and refluxed for 21h.30. Then a second portion of 5 parts of bromocyclopentane is added and stirring at reflux temperature is continued for another 30 hours. The reaction mixture is cooled, filtered and the filtrate is evaporated. The oily residue solidifies on triturating in 1,1'-oxybisethane. The solid product is filtered off and crystallized from 1,1'-oxybisethane, yielding 1.1 parts of N-(4-chlorophenyl)-N-(1-cyclopentyl-4-piperidinyl)benzeneacetamide; mp. 139.5° C.

출처

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