Trifluoroacetic anhydride → Diphenyl-p-tolylsulfonium perfluorooctanesulfonate

HRID 1265964

Reaktionsgleichung

Reaktionsgleichung von HRID 1265964
[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:56])([S:52]([OH:55])(=[O:54])=[O:53])[C:30]([F:51])([F:50])[C:31]([F:49])([F:48])[C:32]([F:47])([F:46])[C:33]([F:45])([F:44])[C:34]([F:43])([F:42])[C:35]([F:41])([F:40])[C:36]([F:39])([F:38])[F:37]>C1(C)C=CC=CC=1>[F:56][C:29]([F:28])([S:52]([O-:55])(=[O:54])=[O:53])[C:30]([F:50])([F:51])[C:31]([F:49])([F:48])[C:32]([F:46])([F:47])[C:33]([F:45])([F:44])[C:34]([F:43])([F:42])[C:35]([F:41])([F:40])[C:36]([F:39])([F:38])[F:37].[CH3:36][C:35]1[CH:30]=[CH:31][C:32]([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:33][CH:34]=1

Komponenten

5

Edukt 3

HCID 9845Trifluoroacetic anhydrideHCID 13679Diphenyl sulfoxideHCID 74483Perfluorooctanesulfonic acid

Produkt 1

HCID 21863659Diphenyl-p-tolylsulfonium perfluorooctanesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
2 °C

Versuchsvorschrift

Into a four-necked flask were charged 8.0 parts of diphenylsulfoxide and 80.0 parts of toluene, and the mixture was cooled to 2° C. Then, 16.6 parts of trifluoroacetic anhydride and 19.8 parts of perfluorooctanesulfonic acid were added and the mixture was stirred at the same temperature for 30 minutes. After standing, the lower layer was concentrated and diluted with 340 parts of chloroform. The obtained chloroform solution was washed six times with 85 parts of ion-exchange water and concentrated to give 27.7 parts of 4-methylphenyldiphenylsulfonium perfluorooctanesulfonate, which is referred to herein as PAG3.

Aufarbeitung

  1. concentrationthe lower layer was concentrated
  2. additiondiluted with 340 parts of chloroform
  3. washThe obtained chloroform solution was washed six times with 85 parts of ion-exchange water
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-e291b3deeda3401d959cef567596a5b2
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06548221B2

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