* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With potassium tert-butylate; In toluene; at 0 - 20℃; for 1.0h;
Example 21; Preparation of compound 190; To a suspension of 20 mg (0.17 mmol) of potassium tert-butanolate in 40 ml of dry toluene is added dropwise under nitrogen at 0°C 4.13 g (17.3 mmol) of 3-mercapto-propyltriethoxysi- lane, followed by the dropwise addition of 5.89 g (17.3 mmol) of <strong>[2915-53-9]dioctyl maleate</strong>. The reaction mixture is stirred for one hour at room temperature. Water is then added and the product is extracted with ethyl acetate. The organic phase is washed with H2O, NaCI, dried over sodium sulfate, filtered and evaporated to dryness using a rotary evaporator to afford 9.80 g of compound 190 as colourless liquid. 1H-NMR (300 MHz, CDCI3): delta = 4.20-4.00 (m, CO2CH2, 4H); 3.90-3.75 (m, SiOCH2, 6H); 3.70-3.60 (m, SCHCO2, 1 H); 3.10-2.95 (m, SCHCH2CO2, 1 H); 2.70-2.60 (m, SCHCH2CO2 + SCH2, 3H); 1.80-1.55 (m, SCH2CH2 + CO2CH2CH2, 6H); 1.55-1.15 (m, SiOCH2CH3 + CH2, 29H); 1.00-0.80 (m, CH3, 6H); 0.80-0.65 (m, SiCH2, 2H).
With 2,2-dimethoxy-2-phenylacetophenone; In methanol; at 20.0℃; for 18.0h;UV-irradiation; Darkness;
Weigh 5mmol γ-mercaptopropyl triethoxysilane in 10mL aluminum foil wrapped quartz round bottom flask, then add 5mmol of 1-vinyl-3-butyl imidazolium hexafluorophosphate ionic liquid, benzoin dimethyl ether And 0.7mL of anhydrous acetonitrile, wherein the amount of benzoin dimethyl ether is 1-vinyl-3-butyl imidazole hexafluorophosphate ionic liquid material amount of 2%; with stirring at 400rpm, purged with argon After 5min, the aluminum foil paper was removed and placed in a 30W UV lamp (365nm) at room temperature for 18h. Then the solvent was removed in a vacuum oven at 40 C to obtain 1.77g of a yellow viscous liquid as the target imidazolium ion Liquid silane coupling agent, yield 73.5%.Referring to FIG. 4, it can be seen from FIG. 4 that the structure of the ionic liquid silane coupling agent prepared in Example 3 is as shown in FIG. 1.