Silicon-containing sulfuric acid ester salt
A technology of sulfate ester salt and sulfate ester, which is applied in the direction of organic chemistry, organic electrolyte, silicon organic compound, etc., to achieve the effect of small environmental load and electrochemical stability
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Embodiment 1
[0107] [Example 1] Synthesis of Silicon-Containing Sulfate Salt 1
[0108] [chemical 10]
[0109]
[0110] 1.0 equivalent of trimethylsilylpropane (manufactured by Sigma-Aldrich), 1.1 equivalent of sulfamic acid (manufactured by Wako Pure Chemical Industries, Ltd.), and 0.2 equivalent of urea (manufactured by Wako Pure Chemical Industries, Ltd.) were placed in a nitrogen atmosphere Mix under pressure and heat to 150°C while stirring. After reaching 150°C, continue stirring and heating for 6 hours, and then allow to cool to room temperature. Ethyl acetate (manufactured by Wako Pure Chemical Industries, Ltd.) was added until the obtained solid was completely immersed, and the solid was pulverized with a spoon or the like, and stirred for about 1 hour, and then the solid was separated by filtration under reduced pressure. its dry. Compound A (yield: 79%) was obtained as the target compound in a state containing some urea.
[0111] [chemical 11]
[0112]
[0113] 1.0 eq...
Embodiment 2
[0114] [Example 2] Synthesis of silicon-containing sulfate ester salt 2
[0115] [chemical 12]
[0116]
[0117] In the same manner as in Example 1, a colorless Silicon-containing sulfate ester salt 2 as a transparent liquid (91% yield). will contain the sulfate salt of silicon 2 1 H-NMR figure (solvent: heavy chloroform) is shown in Figure 4 , plotting the DSC in the Figure 5 , plotting the TG-DTA in Image 6 .
[0118] Table 1 shows the melting point and decomposition point (10% weight loss, under air) of silicon-containing sulfate ester salts 1 to 2 determined by DSC and TG-DTA measurement.
[0119] [Table 1]
[0120]
Embodiment 3、4
[0121] [Example 3, 4] Measurement of Potential Window
[0122] Cyclic voltammetry measurements were performed on silicon-containing sulfate ester salt 1 (Example 3) and silicon-containing sulfate ester salt 2 (Example 4). show the result in Figure 7 (Example 3) and Figure 8 (Example 4). As is clear from these figures, the silicon-containing sulfate ester salt of the present invention has a wide potential window and excellent electrochemical stability.
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