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

HRID 2111496
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HRID 2111496 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매
HCID 962
Water
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fa0325d8cf6c4b4a9b0d31cc5dc19c98
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07521170B2

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