Potassium Iodide → HCID 23339043, 화합물

HRID 2049068노트

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HRID 2049068 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([N:11]([C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=2)[CH:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[O:10])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+].I[CH2:34][CH2:35][CH3:36]>C(O)CCC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([N:11]([C:18]2[CH:19]=[CH:20][C:21]([Cl:24])=[CH:22][CH:23]=2)[CH:12]2[CH2:17][CH2:16][N:15]([CH2:34][CH2:35][CH3:36])[CH2:14][CH2:13]2)=[O:10])=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 336431-Iodopropane2회HCID 233389954-chloro-N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide

생성물 1

HCID 23339043HCID 23339043, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

To a stirred and refluxing mixture of 5 parts of 4-chloro-N-(4-chlorophenyl)-N-(4-piperidinyl)benzeneacetamide, 5 parts of sodium carbonate, 0.4 parts of potassium iodide and 200 parts of butanol is added 4.7 parts of 1-iodopropane and the whole is stirred and refluxed for 22 hours. Then a second portion of 4.5 parts of 1-iodopropane is added and stirring and refluxing is continued for 27 h. 30. The reaction mixture is cooled, filtered and the filtrate is evaporated. The semi-solid residue is dissolved in methylbenzene. The solution is filtered from some impurities and the filtrate is evaporated again. The residue is crystallized from 1,1'-oxybisethane at -10° C., yielding 0.9 parts of 4-chloro-N-(4-chlorophenyl)-N-(1-propyl-4-piperidinyl)benzeneacetamide; mp. 118.6° C.

후처리

  1. temperaturerefluxing
  2. stirringthe whole is stirred
  3. temperaturerefluxed for 22 hours
  4. stirringstirring
  5. temperaturerefluxing
  6. temperatureThe reaction mixture is cooled
  7. filtrationfiltered
  8. customthe filtrate is evaporated
  9. dissolutionThe semi-solid residue is dissolved in methylbenzene
  10. filtrationThe solution is filtered from some impurities
  11. customthe filtrate is evaporated again
  12. customThe residue is crystallized from 1,1'-oxybisethane at -10° C.

출처 및 근거

ORD 기록
ord-8d73890ae34243e082124566c64caccc
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04196210

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