Hydrochloric Acid → Triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate

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Reaktionsgleichung

Br[C:2]([F:10])([F:9])[C:3]([F:8])([F:7])[CH2:4][CH2:5][OH:6].[S:11](S([O-])=O)([O-:13])=[O:12].[Na+].[Na+].[CH2:19]([N:21]([CH2:24][CH3:25])[CH2:22][CH3:23])[CH3:20].Cl>O.C(#N)C>[F:9][C:2]([F:10])([S:11]([O-:13])=[O:12])[C:3]([F:8])([F:7])[CH2:4][CH2:5][OH:6].[CH2:19]([NH+:21]([CH2:24][CH3:25])[CH2:22][CH3:23])[CH3:20]

Komponenten

Reaktionsbedingungen

Temperatur: 60 °C

Versuchsvorschrift

A 1 L reactor was charged with 100.0 g (0.44 mole/1.0 equivalent) of 4-bromo-3,3,4,4-tetrafluorobutan-1-ol, 300 g of acetonitrile, 250 g of water, 108.2 g (0.62 mole/1.4 equivalent) of sodium dithionite and 53.4 g (0.52 mole/1.2 equivalents) of triethylamine, followed by 4 hours of stirring at 60° C. Upon confirming the termination of the reaction, the reaction liquid underwent cooling and 100 mL of 1N HCl was added thereto, followed by stirring. Subsequently, an organic layer was separated, and then the organic layer was subjected to distillation of the solvent, thereby obtaining 264 g of a target triethylammonium 1,1,2,2-tetrafluoro-4-hydroxy-butane-1-sulfinate. It exhibited a purity of 46% and a yield of 88% at this time.

Aufarbeitung

customthe termination of the reaction
customthe reaction liquid underwent
temperaturecooling
stirringby stirring
customSubsequently, an organic layer was separated
distillationthe organic layer was subjected to distillation of the solvent

Quellen und Nachweise

ORD-Eintrag: ord-96823f07e58c450b88a404b7464c34ba
Quelldatensatz: uspto-grants-2015_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09024058B2

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