Dichloromethane → Triphenylsulfonium perfluorooctanesulfonate

HRID 2913

반응식

HRID 2913 반응식
[K+].[F:2][C:3]([F:30])([S:26]([O-:29])(=[O:28])=[O:27])[C:4]([F:25])([F:24])[C:5]([F:23])([F:22])[C:6]([F:21])([F:20])[C:7]([F:19])([F:18])[C:8]([F:17])([F:16])[C:9]([F:15])([F:14])[C:10]([F:13])([F:12])[F:11].[Cl-].[C:32]1([S+:38]([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)[C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.ClCCl>O>[F:30][C:3]([F:2])([S:26]([O-:29])(=[O:28])=[O:27])[C:4]([F:24])([F:25])[C:5]([F:23])([F:22])[C:6]([F:20])([F:21])[C:7]([F:19])([F:18])[C:8]([F:17])([F:16])[C:9]([F:15])([F:14])[C:10]([F:13])([F:12])[F:11].[C:45]1([S+:38]([C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)[C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[CH:46]=[CH:47][CH:48]=[CH:49][CH:50]=1

참가 물질

5

반응물 3

HCID 6344Dichloromethane2회HCID 61343Triphenylsulfonium chlorideHCID 23669238Potassium perfluorooctanesulfonate

생성물 1

HCID 21863781Triphenylsulfonium perfluorooctanesulfonate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a suspension of perfluorooctanesulfonic acid potassium salt (24.64 g, 46.1 mmol) in water (150 ml) at room temperature under nitrogen was added dropwise triphenylsulfonium chloride (50% aqueous solution, 27.50 g) over 15 minutes. After stirring the suspension for 30 minutes, dichloromethane (75 ml) was added and the mixture stirred at room temperature for 20 hours. Additional dichloromethane (225 ml) was added and the layers separated. The organic layer was washed with water (5×125 ml) until the washings were neutral (pH 7 ). After drying (MgSO4 ), removal of the solvent in vacuo gave a viscous gum which was further dried by heating at 80°-90° C. for 84 hours under vacuum. In this way, triphenylsulfonium perfluorooctanesulfonate was isolated as a glassy solid (30.61 g).

후처리

  1. stirringthe mixture stirred at room temperature for 20 hours
  2. customthe layers separated
  3. washThe organic layer was washed with water (5×125 ml) until the washings
  4. customAfter drying
  5. custom(MgSO4 ), removal of the solvent in vacuo
  6. customgave a viscous gum which
  7. customwas further dried
  8. temperatureby heating at 80°-90° C. for 84 hours under vacuum

출처 및 근거

ORD 기록
ord-d1e6e90adf2744bfa6b435f6c7114ace
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731364

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