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Water → HCID 86736100, 화합물

HRID 1112410
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HRID 1112410 반응식
Cl[CH2:2][CH2:3][CH2:4][CH:5]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7].[N:21]1[CH:26]=[CH:25][C:24]([CH2:27][N:28]2[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)=[CH:23][CH:22]=1.[C:34](=[O:37])([O-])[O-:35].[Na+].[Na+].[C:40]1([CH3:46])C=CC=C[CH:41]=1.[OH2:47]>>[C:34]([OH:35])(=[O:37])/[CH:24]=[CH:23]\[C:22]([OH:7])=[O:47].[C:34]([OH:35])(=[O:37])/[CH:41]=[CH:40]\[C:46]([OH:7])=[O:47].[C:34]([OH:35])(=[O:37])/[CH:24]=[CH:23]\[C:22]([OH:7])=[O:47].[C:15]1([CH:5]([S:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)(=[O:8])=[O:7])[CH2:4][CH2:3][CH2:2][N:31]2[CH2:32][CH2:33][N:28]([CH2:27][C:24]3[CH:23]=[CH:22][N:21]=[CH:26][CH:25]=3)[CH2:29][CH2:30]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 962WaterHCID 1140TolueneHCID 10340Sodium CarbonateHCID 8087151-((Pyridin-4-yl)methyl)piperazineHCID 22763811[1-(Benzenesulfonyl)-4-chlorobutyl]benzene

생성물 1

HCID 86736100HCID 86736100, 화합물

실험 절차

A mixture of 6.16 g of 1-chloro-4-phenyl-4-phenylsulfonylbutane, 4.25 g of 4-(4-pyridylmethyl)piperazine, 4.24 g of sodium carbonate and 80 ml of toluene was refluxed with stirring for 72 hours. After cooling, water was added to the reaction mixture and the toluene layer was separated. The eoluene layer was extracted with a 10% aqueous hydrochloric acid solution and neutralized with potassium carbonate and then extracted with ethyl acetate. After drying over potassium carbonate, to the extract was added 7.0 g of maleic acid. The resulting maleate was purified with 2-propanol to give 3 g of 1-(4-phenyl-4-phenylsulfonylbutyl)-4-(4-pyridylmethyl)piperazine trimaleate, melting at 144°-146° C with decomposition.

후처리

  1. temperaturewas refluxed
  2. temperatureAfter cooling
  3. customthe toluene layer was separated
  4. extractionThe eoluene layer was extracted with a 10% aqueous hydrochloric acid solution
  5. extractionextracted with ethyl acetate
  6. dry with materialAfter drying over potassium carbonate, to the extract
  7. additionwas added 7.0 g of maleic acid
  8. customThe resulting maleate was purified with 2-propanol

출처 및 근거

ORD 기록
ord-2f607a88a5834387a99d9453731ce909
출처 데이터셋
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04122178

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