Chloroform → Bis(triphenylsulfonium) perfluorobutane-1,4-disulfonate

HRID 414881

反応式

HRID 414881 の反応式
[K+].[F:2][C:3]([F:21])([S:17]([O-:20])(=[O:19])=[O:18])[C:4]([F:16])([F:15])[C:5]([F:14])([F:13])[C:6]([F:12])([F:11])[S:7]([O-:10])(=[O:9])=[O:8].[K+].[Br-].[C:24]1([S+:30]([C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(Cl)(Cl)Cl>O>[F:12][C:6]([F:11])([S:7]([O-:10])(=[O:9])=[O:8])[C:5]([F:14])([F:13])[C:4]([F:15])([F:16])[C:3]([F:2])([F:21])[S:17]([O-:20])(=[O:18])=[O:19].[C:37]1([S+:30]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=1.[C:37]1([S+:30]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=1

参加物

5

反応物 3

HCID 6212ChloroformHCID 11984010Triphenylsulfonium BromideHCID 14384439Perfluorobutane-1,4-disulfonic acid potassium salt

生成物 1

HCID 87079447Bis(triphenylsulfonium) perfluorobutane-1,4-disulfonate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Perfluorobutane-1,4-disulfonic acid potassium salt (2.5 g) was added to a solution of triphenylsulfonium bromide (3.5 g) in 150 ml of water. Chloroform (150 ml) was added and stirred for 5 hours. The chloroform layer was washed several times with water, dried over anhydrous sodium sulfate, filtered, and the filtrate evaporated to an oil stage. Ether was added to the oil and the mixture was stirred vigorously. A white precipitate formed. The mixture was filtered and recovered precipitate was dried under vacuum, resulting in a white powder; mp 155° C.

後処理

  1. washThe chloroform layer was washed several times with water
  2. dry with materialdried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. customthe filtrate evaporated to an oil stage
  5. additionEther was added to the oil
  6. stirringthe mixture was stirred vigorously
  7. customA white precipitate formed
  8. filtrationThe mixture was filtered
  9. customrecovered precipitate
  10. customwas dried under vacuum
  11. customresulting in a white powder

出典と根拠

ORDレコード
ord-5a8415d00d4646b4972e7d00f9d6914e
出典データセット
uspto-grants-2012_01
特許番号
US08088548B2

関連ノート

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