Sulfur tetrafluoride → Perfluoro-3-(butoxy)propene

HRID 1680424

Reaktionsgleichung

Reaktionsgleichung von HRID 1680424
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Komponenten

6

Edukt 4

HCID 24555Sulfur tetrafluorideHCID 67632Heptafluorobutyroyl fluorideHCID 522689Potassium FluorideHCID 2776028Pentafluoroallyl fluorosulphate

Produkt 1

HCID 54369168Perfluoro-3-(butoxy)propeneAusbeute 64 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8150DiglymeLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

A mixture of dry potassium fluoride (7.50 g, 0.13 mol), diglyme (100 ml) and heptafluorobutyroyl fluoride (prepared from the acid by treatment with sulfur tetrafluoride) (28.1 g, 0.13 mol) was stirred at 5° C. for 30 min. Perfluoroallyl fluorosulfate was added dropwise at 5° C., the mixture was stirred at this temperature for 1 hour, then at 25° C. for 3 hours. The volatile components were transferred by distillation at 40° C. (8 mm Hg), washed with water (100 ml), and distilled from a small amount of concentrated sulfuric acid to give perfluoro-3-(butoxy)propene (30.3 g, 0.083 mol, 64%) bp 80°-84° C. whose structure was confirmed by:

Aufarbeitung

  1. stirringthe mixture was stirred at this temperature for 1 hour
  2. waitat 25° C. for 3 hours
  3. distillationThe volatile components were transferred by distillation at 40° C. (8 mm Hg)
  4. washwashed with water (100 ml)
  5. distillationdistilled from a small amount of concentrated sulfuric acid

Quellen und Nachweise

ORD-Eintrag
ord-583dc2b02951406291c442ca2545b358
Quelldatensatz
uspto-grants-1981_06
Patentnummer
US04273729

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