Sodium perfluorobutanesulfonate → HCID 178448399, Verbindung

HRID 1168023Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1168023
C(OP([O-])(OCC)=O)C.[C:10]([IH+:14]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([CH3:13])([CH3:12])[CH3:11].[F:25][C:26]([F:41])([S:37]([O-:40])(=[O:39])=[O:38])[C:27]([F:36])([F:35])[C:28]([F:34])([F:33])[C:29]([F:32])([F:31])[F:30].[Na+]>O>[F:41][C:26]([F:25])([S:37]([O-:40])(=[O:39])=[O:38])[C:27]([F:35])([F:36])[C:28]([F:34])([F:33])[C:29]([F:32])([F:31])[F:30].[C:21]([IH+:14]([C:10]([CH3:13])([CH3:12])[CH3:11])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([CH3:24])([CH3:23])[CH3:22]

Komponenten

4

Edukt 2

HCID 23678450Sodium perfluorobutanesulfonateHCID 178448396HCID 178448396, Verbindung

Produkt 1

HCID 178448399HCID 178448399, VerbindungAusbeute 90,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Di-tert-butylphenyliodonium diethylphosphate (546 mg; 1 mmol) and sodium perfluorobutanesulfonate (354 mg; 1.1 mmol) were dissolved in water (10 ml), and the resultant mixture was extracted three times with methylene chloride (10 ml). The solvent was removed through distillation, and precipitated white solid was washed with ether, followed by recrystallization from a mixture of methylene chloride and ether, to thereby precipitate 561 mg of the target compound as white crystals (yield: 81%).

Aufarbeitung

  1. extractionthe resultant mixture was extracted three times with methylene chloride (10 ml)
  2. customThe solvent was removed through distillation
  3. customprecipitated white solid
  4. washwas washed with ether
  5. customfollowed by recrystallization from a mixture of methylene chloride and ether

Quellen und Nachweise

ORD-Eintrag
ord-6f78140de4bd437eadeadc7a1aa1a9ea
Quelldatensatz
uspto-grants-2003_09
Patentnummer
US06620957B1

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