Difluoro(fluorosulphonyl)acetyl fluoride → CH2=C(CF2Ocf2CF2SO2F)2

HRID 492277

Reaktionsgleichung

Reaktionsgleichung von HRID 492277
[CH2:1]=[C:2]([C:11](OS(F)(=O)=O)([F:13])[F:12])[C:3]([O:6][S:7]([F:10])(=[O:9])=[O:8])([F:5])[F:4].[F:19][S:20]([C:23]([C:26]([O:29][K])([F:28])[F:27])([F:25])[F:24])(=[O:22])=[O:21].[F-:31].[K+].[F:33][S:34]([C:37]([C:40]([F:42])=[O:41])([F:39])[F:38])(=[O:36])=[O:35]>COCCOCCOC.O>[CH2:1]=[C:2]([C:3]([O:6][S:7]([F:10])(=[O:9])=[O:8])([F:5])[F:4])[C:11]([F:13])([F:19])[F:12].[CH2:1]=[C:2]([C:11]([O:41][C:40]([C:37]([S:34]([F:33])(=[O:36])=[O:35])([F:39])[F:38])([F:31])[F:42])([F:13])[F:12])[C:3]([O:29][C:26]([C:23]([S:20]([F:19])(=[O:22])=[O:21])([F:25])[F:24])([F:28])[F:27])([F:5])[F:4]

Komponenten

8

Edukt 4

HCID 69614Difluoro(fluorosulphonyl)acetyl fluorideHCID 522689Potassium FluorideHCID 10471472CH2=C(CF2Oso2F)2HCID 178527443HCID 178527443, Verbindung

Produkt 2

HCID 87741755CH2=C(CF3)CF2Oso2FHCID 131726625CH2=C(CF2Ocf2CF2SO2F)2Ausbeute 58 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8150DiglymeLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

CH2═C(CF2OSO2F)2 is added gradually to FSO2CF2CF2OK, which is prepared from freshly dried KF (3.9 g, 0.067 mole) and FSO2CF2COF (12 g, 0.067 mole) in dry diglyme (30 ml). The resulting mixture is stirred 3 hours at 20° C. The reaction mixture is poured into water. The organic layer is washed with aqueous sodium bicarbonate, then water, and then dried over MgSO4. Distillation gives CH2═C(CF3)CF2OSO2F (0.5 g) and CH2═C(CF2OCF2CF2SO2F)2 (9 g, 58% yield, b.pt. 95-96° C. at 15 mm Hg).

Aufarbeitung

  1. washThe organic layer is washed with aqueous sodium bicarbonate
  2. dry with materialwater, and then dried over MgSO4
  3. distillationDistillation

Quellen und Nachweise

ORD-Eintrag
ord-daa31aa198fd43f28910e7fc0418ebc5
Quelldatensatz
uspto-grants-2009_05
Patentnummer
US07531689B2

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