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Chloroform → Bis(tris(4-t-butylphenyl)sulfonium) perfluorobutane-1,4-disulfonate

HRID 2111496
ノート
印刷プレビュー

反応式

HRID 2111496 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+].[OH-].[C:24]([C:28]1[CH:33]=[CH:32][C:31]([S+:34]([C:45]2[CH:50]=[CH:49][C:48]([C:51]([CH3:54])([CH3:53])[CH3:52])=[CH:47][CH:46]=2)[C:35]2[CH:40]=[CH:39][C:38]([C:41]([CH3:44])([CH3:43])[CH3:42])=[CH:37][CH:36]=2)=[CH:30][CH:29]=1)([CH3:27])([CH3:26])[CH3:25].C(Cl)(Cl)Cl>O.CC(C)=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:24]([C:28]1[CH:33]=[CH:32][C:31]([S+:34]([C:35]2[CH:40]=[CH:39][C:38]([C:41]([CH3:44])([CH3:43])[CH3:42])=[CH:37][CH:36]=2)[C:45]2[CH:50]=[CH:49][C:48]([C:51]([CH3:53])([CH3:54])[CH3:52])=[CH:47][CH:46]=2)=[CH:30][CH:29]=1)([CH3:25])([CH3:26])[CH3:27].[C:24]([C:28]1[CH:33]=[CH:32][C:31]([S+:34]([C:35]2[CH:40]=[CH:39][C:38]([C:41]([CH3:44])([CH3:43])[CH3:42])=[CH:37][CH:36]=2)[C:45]2[CH:50]=[CH:49][C:48]([C:51]([CH3:53])([CH3:54])[CH3:52])=[CH:47][CH:46]=2)=[CH:30][CH:29]=1)([CH3:25])([CH3:26])[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6212ChloroformHCID 14384439Perfluorobutane-1,4-disulfonic acid potassium saltHCID 87569163Tris(4-t-butylphenyl)sulfonium hydroxide

生成物 1

HCID 87388084Bis(tris(4-t-butylphenyl)sulfonium) perfluorobutane-1,4-disulfonate

試薬・触媒・溶媒 2

HCID 180Acetone溶媒
HCID 962
Water
溶媒

実験手順

Perfluorobutane-1,4-disulfonic acid potassium salt (2.92 g) in 100 ml water was added to a solution of tris(4-t-butylphenyl)sulfonium hydroxide (7.75 g) in 150 ml of acetone. 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 the recovered precipitate was dried under vacuum, resulting in a white powder; mp 190° 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. customthe recovered precipitate was dried under vacuum
  10. customresulting in a white powder

出典と根拠

ORDレコード
ord-fa0325d8cf6c4b4a9b0d31cc5dc19c98
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07521170B2

反応ノート

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