Toluene → Diphenyl(4-methylphenyl)sulfonium nonafluorobutanesulfonate

HRID 1934293

반응식

HRID 1934293 반응식
[C:1]1([S:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.[F:28][C:29]([F:44])([S:40]([OH:43])(=[O:42])=[O:41])[C:30]([F:39])([F:38])[C:31]([F:37])([F:36])[C:32]([F:35])([F:34])[F:33].[C:45]1([CH3:51])[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=1>>[F:44][C:29]([F:28])([S:40]([O-:43])(=[O:42])=[O:41])[C:30]([F:38])([F:39])[C:31]([F:37])([F:36])[C:32]([F:35])([F:34])[F:33].[CH3:51][C:45]1[CH:50]=[CH:49][C:48]([S+:7]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:47][CH:46]=1

참가 물질

5

반응물 4

HCID 1140TolueneHCID 9845Trifluoroacetic anhydrideHCID 13679Diphenyl sulfoxideHCID 67815Perfluorobutanesulfonic acid

생성물 1

HCID 21863628Diphenyl(4-methylphenyl)sulfonium nonafluorobutanesulfonate

반응 조건

온도
2 °C

실험 절차

Into a four-necked flask were charged 5.06 parts of diphenylsulfoxide and 50.6 parts of toluene, and the mixture was cooled to 2° C. Then, 10.5 parts of trifluoroacetic anhydride and 7.50 parts of perfluorobutanesulfonic acid were added and the mixture was stirred at the same temperature for 60 minutes. After standing, the lower layer was concentrated and diluted with 100 parts of chloroform. The obtained chloroform solution was washed 11 times with 50 parts of ion-exchange water and concentrated to give 12.0 parts of 4-methylphenyldiphenylsulfonium perfluorobutanesulfonate, which is referred to herein as PAG4.

후처리

  1. concentrationthe lower layer was concentrated
  2. additiondiluted with 100 parts of chloroform
  3. washThe obtained chloroform solution was washed 11 times with 50 parts of ion-exchange water
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cb9cd00415714cfdadc5e0a42fc263c9
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06383713B1

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