تفاعل #420293

معادلة التفاعل

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

hydrogen peroxide water

→

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

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   أخرىA glass flask equipped with a thermometer, a condenser and a dropping funnel
2. 2
   أخرىobtained by Comparative Example 1-2
3. 3
   أخرىAfter terminating the dropping
4. 4
   workup.STIRRINGstirring
5. 5
   تركيزAfter concentrating
6. 6
   أخرىthe reaction liquid, it
7. 7
   غسيلwas washed with 10 ml of diisopropyl ether
8. 8
   ترشيحfollowed by filtration
9. 9
   أخرىdrying the obtained solid matter

الإجراء التجريبي

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.

المصدر