반응 #55033
ord-0fb7ca53bca64e0fa512792348c1f012
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시약
반응 조건
후처리
- 1온도warm
- 2workup.STIRRINGthe whole is stirred
- 3온도refluxed for 21h.30
- 4workup.STIRRINGstirring
- 5온도at reflux temperature
- 6온도The reaction mixture is cooled
- 7여과filtered
- 8기타the filtrate is evaporated
- 9기타on triturating in 1,1'-oxybisethane
- 10여과The solid product is filtered off
- 11기타crystallized 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.