Heptafluorobutyric acid → HCID 22328343, Verbindung

HRID 584039

Reaktionsgleichung

Reaktionsgleichung von HRID 584039
FC(F)(F)S([O-])(=O)=O.[C:9]1([S+:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[F:28][C:29]([F:40])([F:39])[C:30]([F:38])([F:37])[C:31]([F:36])([F:35])[C:32]([OH:34])=[O:33]>CO.C[N+](C)(C)C.[Cl-]>[F:28][C:29]([F:39])([F:40])[C:30]([F:37])([F:38])[C:31]([F:35])([F:36])[C:32]([O-:34])=[O:33].[C:22]1([S+:15]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

Komponenten

5

Edukt 2

HCID 9777Heptafluorobutyric acidHCID 11729320Sulfonium, triphenyl-, 1,1,1-trifluoromethanesulfonate (1:1)

Produkt 1

HCID 22328343HCID 22328343, VerbindungAusbeute 119,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6379Tetramethylammonium chlorideKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

In aqueous methanol solution were dissolved 20.6 g (50 mmol) of the resulting triphenylsulfonium trifluoromethanesulfonate, and passed through an activated strong base type anion exchange resin (Amberlite IRA-900 by Organo Corp.). To the elutant solution was added 24.8 g (60 mmol) of heptafluorobutyric acid and allowed reacting with stirring at room temperature for 1 hour. After completion of the reaction, the solvent was removed and the residue was dissolved in 200 ml methylene chloride, washed with water 3 times and concentrated under reduced pressure to give 28.4 g (yield: 84%) of triphenylsulfonium heptafluorobutanoate as a white crystal.

Aufarbeitung

  1. customAfter completion of the reaction
  2. customthe solvent was removed
  3. dissolutionthe residue was dissolved in 200 ml methylene chloride
  4. washwashed with water 3 times
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6837c286a7ce4d37b3d50fd655588b40
Quelldatensatz
uspto-grants-2005_08
Patentnummer
US06924323B2

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