Dichloromethane → Triphenylsulfonium perfluorooctanesulfonate

HRID 1794974ノート

反応式

HRID 1794974 の反応式
[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].[Br-].[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

参加物

5

反応物 3

HCID 6344Dichloromethane2 回HCID 11984010Triphenylsulfonium BromideHCID 23669238Potassium perfluorooctanesulfonate

生成物 1

HCID 21863781Triphenylsulfonium perfluorooctanesulfonate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

To a suspension of perfluorooctanesulfonic acid potassium salt (10.76 g, 20.0 mmol) in water (100 mL) at room temperature under nitrogen was added dropwise triphenylsulfonium bromide (6.87 g, 20.0 mmol) over 15 min. After stirring the suspension for 30 min., dichloromethane (100 mL) was added and the biphasic mixture stirred at room temperature for 20 hours. Additional dichloromethane (100 mL) was added and the layers separated. The organic layer was washed with water (3×75 mL) until the washings were neutral (pH 7). After drying (MgSO4), removal of the solvent in vacuum gave a viscous gum which was further dried by heating at 50° C. for 24 hours under vacuum. In this way, triphenylsulfonium perfluorooctanesulfonate was isolated as a pale yellow gummy solid.

後処理

  1. stirringthe biphasic mixture stirred at room temperature for 20 hours
  2. customthe layers separated
  3. washThe organic layer was washed with water (3×75 mL) until the washings
  4. customAfter drying
  5. custom(MgSO4), removal of the solvent in vacuum
  6. customgave a viscous gum which
  7. customwas further dried

出典と根拠

ORDレコード
ord-47b048caa6be466fa610fe7bd4c52d6e
出典データセット
uspto-grants-2006_04
特許番号
US07026093B2

反応ノート

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