Reaktion #420293

Reaktionsgleichung

sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfinate

hydrogen peroxide water

→

sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfonate

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA glass flask equipped with a thermometer, a condenser and a dropping funnel
2. 2
   Sonstigeobtained by Comparative Example 1-2
3. 3
   SonstigeAfter terminating the dropping
4. 4
   workup.STIRRINGstirring
5. 5
   EinengenAfter concentrating
6. 6
   Sonstigethe reaction liquid, it
7. 7
   Waschenwas washed with 10 ml of diisopropyl ether
8. 8
   Filtrationfollowed by filtration
9. 9
   Sonstigedrying the obtained solid matter

Vorschrift

A glass flask equipped with a thermometer, a condenser and a dropping funnel was charged with 10.0 g (10.5 mmol) of sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfinate having a purity of 39% obtained by Comparative Example 1-2, a catalytic amount of sodium tungstate dihydrate, and 10 ml of water, followed by stirring. Then, 2.4 g (21.0 mmol) of 30% hydrogen peroxide water was added dropwise in an ice bath. After terminating the dropping, stirring was continued at room temperature for one hour. The reaction termination was confirmed by 19F NMR. After concentrating the reaction liquid, it was washed with 10 ml of diisopropyl ether, followed by filtration and drying the obtained solid matter. After that, there was obtained as a white-color solid matter 9.1 g (yield 90%, purity 40%) of sodium 1,1,2,2-tetrafluoro-6-cyclohexylcarbonyloxyhexane-1-sulfonate. Upon this, 7% of 6-bromo-5,5,6,6-tetrafluorohexane cyclohexanecarboxylate was produced as a by-product.

Quelle