反应 #420293

反应方程式

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

hydrogen peroxide water

→

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

溶剂

water

反应条件

后处理

1. 1
   其他A glass flask equipped with a thermometer, a condenser and a dropping funnel
2. 2
   其他obtained by Comparative Example 1-2
3. 3
   其他After terminating the dropping
4. 4
   workup.STIRRINGstirring
5. 5
   浓缩After concentrating
6. 6
   其他the reaction liquid, it
7. 7
   洗涤was washed with 10 ml of diisopropyl ether
8. 8
   过滤followed by filtration
9. 9
   其他drying the obtained solid matter

实验过程

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.

来源