تفاعل #55033

ord-0fb7ca53bca64e0fa512792348c1f012

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwarm
  2. 2
    workup.STIRRINGthe whole is stirred
  3. 3
    درجة الحرارةrefluxed for 21h.30
  4. 4
    workup.STIRRINGstirring
  5. 5
    درجة الحرارةat reflux temperature
  6. 6
    درجة الحرارةThe reaction mixture is cooled
  7. 7
    ترشيحfiltered
  8. 8
    أخرىthe filtrate is evaporated
  9. 9
    أخرىon triturating in 1,1'-oxybisethane
  10. 10
    ترشيحThe solid product is filtered off
  11. 11
    أخرىcrystallized from 1,1'-oxybisethane

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04151286uspto-grants-1979_04