Hydrogen Peroxide → Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfonate

HRID 571159Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 571159
[F:1][C:2]([F:12])([S:9]([O-:11])=[O:10])[C:3]([F:8])([F:7])[CH2:4][CH2:5][OH:6].[CH2:13]([NH+:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[CH3:14].OO.S([O-])([O-])=[O:23].[Na+].[Na+]>O>[F:12][C:2]([F:1])([S:9]([O-:23])(=[O:11])=[O:10])[C:3]([F:7])([F:8])[CH2:4][CH2:5][OH:6].[CH2:13]([NH+:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[CH3:14]

Komponenten

5

Edukt 3

HCID 784Hydrogen PeroxideHCID 24437Sodium SulfiteHCID 86660801Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate

Produkt 1

HCID 86660802Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfonateAusbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

A 500 mL reactor was charged with 112 g (46% purity, 0.17 moles) of triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate, 200 g of water and 41 g (0.36 mole) of 30% hydrogen peroxide, at room temperature, followed by 6 hours of stirring at 40° C. Upon confirming the termination of the reaction, a reaction liquid underwent cooling and 7.5 g of sodium sulfite was added to the reaction liquid, followed by stirring. Subsequently, a liquid obtained by distilling the solvent out of the reaction liquid was rinsed with 50 g of hexane, and then extracted with 100 g of chloroform. It was heated under a reduced pressure so as to distill a volatile component off and then dried, thereby obtaining 43 g of a target triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfonate. It exhibited a purity of 50% and a yield of 40% at this time. As a result of analysis, it was found that 4-bromo-3,3,4,4-tetrafluorobutan-1-ol which had been confirmed to disappear by the 1st step (sulfination step) was formed during this 2nd step (oxidation step) as a by-product in an amount of 9%.

Aufarbeitung

  1. customthe termination of the reaction
  2. customa reaction liquid underwent
  3. temperaturecooling
  4. stirringby stirring
  5. customSubsequently, a liquid obtained
  6. distillationby distilling the solvent
  7. customout of the reaction liquid
  8. washwas rinsed with 50 g of hexane
  9. extractionextracted with 100 g of chloroform
  10. temperatureIt was heated under a reduced pressure so as
  11. distillationto distill a volatile component off and
  12. customthen dried

Quellen und Nachweise

ORD-Eintrag
ord-92b35a89a4b745bdb2da17a5e1bddf7a
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09024058B2

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