Dimethyl Sulfate → Methyl perfluorobutyl ether

HRID 1634158

Reaktionsgleichung

Reaktionsgleichung von HRID 1634158
[F-:1].[K+].[F:3][C:4]([F:15])([C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10])[C:5]([F:7])=O.S([O:21][CH3:22])(OC)(=O)=O>CN(C)C=O>[C:5]([O:21][CH3:22])([C:4]([C:8]([C:9]([F:12])([F:11])[F:10])([F:14])[F:13])([F:15])[F:3])([F:1])[F:7]

Komponenten

5

Edukt 3

HCID 6497Dimethyl SulfateHCID 67632Heptafluorobutyroyl fluorideHCID 522689Potassium Fluoride

Produkt 1

HCID 164514Methyl perfluorobutyl etherAusbeute 134,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The reaction was carried out in the same equipment and in a similar manner to the procedure of Example 7 above, but using the following materials: spray-dried potassium fluoride (6 kg, 103.1 mole), anhydrous dimethyl formamide (25.1 kg), perfluorobutyryl fluoride (58% purity, 25.1 kg, 67.3 mole), and dimethyl sulfate (12.0 kg, 95.1 mole). 22.6 kg of product was obtained, which was 63.2% C4F9COH3 (b.=58-60° C.). The product identity was confirmed by GCMS and by 1H and 19F NMR.

Quellen und Nachweise

ORD-Eintrag
ord-50c094f998ff4e20890aa27368f7bd32
Quelldatensatz
uspto-grants-2003_01
Patentnummer
US06506459B2

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