Potassium Iodide → N-(4-chlorophenyl)-N-(1-cyclopentyl-4-piperidinyl)benzeneacetamide

HRID 26755

反応式

HRID 26755 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)[C:9](=[O:17])[CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+].Br[CH:33]1[CH2:37][CH2:36][CH2:35][CH2:34]1>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]([CH:18]2[CH2:23][CH2:22][N:21]([CH:33]3[CH2:37][CH2:36][CH2:35][CH2:34]3)[CH2:20][CH2:19]2)[C:9](=[O:17])[CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:6][CH:7]=1

参加物

5

反応物 4

HCID 4875Potassium IodideHCID 8728Bromocyclopentane2 回HCID 10340Sodium CarbonateHCID 162188N-(4-Chlorophenyl)-N-4-piperidinylbenzeneacetamide

生成物 1

HCID 20334078N-(4-chlorophenyl)-N-(1-cyclopentyl-4-piperidinyl)benzeneacetamide

実験手順

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.

後処理

  1. temperaturewarm
  2. stirringthe whole is stirred
  3. temperaturerefluxed for 21h.30
  4. stirringstirring
  5. temperatureat reflux temperature
  6. temperatureThe reaction mixture is cooled
  7. filtrationfiltered
  8. customthe filtrate is evaporated
  9. customon triturating in 1,1'-oxybisethane
  10. filtrationThe solid product is filtered off
  11. customcrystallized from 1,1'-oxybisethane

出典と根拠

ORDレコード
ord-0fb7ca53bca64e0fa512792348c1f012
出典データセット
uspto-grants-1979_04
特許番号
US04151286

関連ノート

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