O-benzyldiethoxymethylsilane and preparation method thereof
A technology of o-benzyldiethoxymethylsilane and benzyldiethoxymethylsilane, applied in chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, organic chemistry, etc., It can solve the problems of solvent environmental pollution and solvent recycling, and achieve the effect of simple separation and purification, saving operating costs and simple process.
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Embodiment 1
[0023] In a dry 250mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 163.4g (0.9214 moles) of methyltriethoxysilane, and add 10.8g (0.4698 moles) of new Cut the sodium flakes, raise the temperature to 103°C, and beat the sodium flakes into sodium sand; within 1 hour, add 29.2g (0.2307 moles) of o-chlorotoluene into the reaction system dropwise through a constant pressure dropping funnel, and control the reaction temperature between 102~104°C, continue to react for 2 hours after the dropwise addition, after cooling to 25°C, slowly add 1.5g (0.0326 moles) of absolute ethanol within 0.5h to neutralize the excess metal sodium, and then add Maintain at 25°C for 1 h; then add 9.4 mL (0.0805 mol) of methyltrichlorosilane dropwise to the mixture within 1 h to neutralize the generated sodium alkoxide; after the addition is complete, continue the reaction at this temperature for 3 h. Then the reaction mixture was suction-filt...
Embodiment 2
[0026] In a dry 250mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 163.8g (0.9187 moles) of methyltriethoxysilane, and add 10.6g (0.4611 moles) of new Cut the sodium flakes, raise the temperature to 95°C, and beat the sodium flakes into sodium sand; within 2 hours, add 29.2g (0.2307 moles) of o-chlorotoluene dropwise into the reaction system through a constant pressure dropping funnel, and control the reaction temperature between 95~98°C, continue to react for 4 hours after the dropwise addition, after cooling to 30°C, slowly add 3.1g (0.0673 moles) of absolute ethanol within 1.0h to neutralize the excess metallic sodium, and then add Maintain at 30°C for 1.5h; then add 9.4mL (0.0805mol) methyltrichlorosilane dropwise to the mixture within 2h to neutralize the generated sodium alkoxide; after the dropwise addition, continue the reaction at this temperature for 4h . Then the reaction mixture was suction-filtered u...
Embodiment 3
[0029] In a dry 250mL four-necked flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 81.9g (0.4593 moles) of methyltriethoxysilane, and add 10.8g (0.4698 moles) of new Cut the sodium flakes, raise the temperature to 95°C, and beat the sodium flakes into sodium sand; within 6 hours, add 29.2g (0.2307 moles) of o-chlorotoluene into the reaction system dropwise through a constant pressure dropping funnel, and control the reaction temperature between 95~98°C, continue to react for 5 hours after the dropwise addition, after cooling to 20°C, slowly add 5.0g (0.1085 moles) of absolute ethanol within 1.0h to neutralize the excess metal sodium, and then add Maintain at 20°C for 1.5h; then add 16.0mL (0.1327mol) dimethyldichlorosilane dropwise to the mixture within 1.5h to neutralize the generated sodium alkoxide; after the addition is complete, continue at this temperature Reaction 2h. Then the reaction mixture was suction-filtered under...
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