Organosilicon compound and synthesis method thereof
A technology of organosilicon compounds and synthesis methods, which is applied in the fields of silicon organic compounds, organic chemistry, chemical instruments and methods, etc., and can solve problems such as unfriendly to the environment, difficulty in realizing functional groups, and uneconomical atoms
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Embodiment 1
[0042] (E)-N-(2,3,5,6-tetrafluoro-4-(trifluoromethyl)phenyl)-2-((1-(2-(trimethylsilyl)phenyl)phenylene Ethyl) amino) oxygen) acetamide synthesis:
[0043] Accurately weigh (E)-2-(((1-phenylethylidene)amino)oxy)-N-(2,3,5,6-tetrafluoro-4-(trifluoromethyl)phenyl) The acetamide reactant (0.05mmol, 20.4mg) was transferred to the reaction vessel, and hexamethyldisilane (0.15mmol, 33μL), PdCl 2 (MeCN) 2(10%mmol, 1.2mg), silver fluoride (0.1mmol, 27.4mg), copper trifluoroacetate (20mmol%, 3mg), lithium fluoride (0.1mmol, 2.4mg), add dropwise 1.0mL trifluorotoluene in In a thick-walled pressure-resistant tube, tighten the stopper of the reaction tube to seal the reaction system, heat to 100°C, and react for 7 hours under the condition of stirring in an oil bath. After the reaction, the reaction solution was cooled to room temperature, filtered through short silica gel to remove insoluble impurities, washed with ethyl acetate, and the solvent was removed from the organic phase to obt...
Embodiment 2
[0045] (E)-2-((1-(4-chloro-2-(trimethylsilyl)phenyl)ethylidene)amino)oxy)-N-(2,3,5,6-tetrafluoro -Synthesis of 4-(trifluoromethyl)phenyl)acetamide:
[0046] Accurately weigh (E)-2-((1-(4-chlorophenyl)ethylidene)amino)oxy)-N-(2,3,5,6-tetrafluoro-4-(trifluoromethyl Base) phenyl) acetamide reactant (0.05mmol, 22.1mg), transfer to reaction vessel, add hexamethyldisilane (0.15mmol, 33μL), PdCl 2 (MeCN) 2 (10%mmol, 1.2mg), silver fluoride (0.1mmol, 27.4mg), copper trifluoroacetate (20mmol%, 3mg), lithium fluoride (0.1mmol, 2.4mg), add dropwise 1.0mL trifluorotoluene in In a thick-walled pressure-resistant tube, tighten the stopper of the reaction tube to seal the reaction system, heat to 100°C, and react for 7 hours under the condition of stirring in an oil bath. After the reaction, the reaction solution was cooled to room temperature, filtered through short silica gel to remove insoluble impurities, washed with ethyl acetate, and the solvent was removed from the organic phase to...
Embodiment 3
[0048] (E)-2-((1-(3-chloro-2-(trimethylsilyl)phenyl)ethylidene)amino)oxy)-N-(2,3,5,6-tetrafluoro -Synthesis of 4-(trifluoromethyl)phenyl)acetamide:
[0049] Accurately weigh (E)-2-((1-(3-chlorophenyl)ethylidene)amino)oxy)-N-(2,3,5,6-tetrafluoro-4-(trifluoromethyl Base) phenyl) acetamide reactant (0.05mmol, 22.1mg), transfer to reaction vessel, add hexamethyldisilane (0.15mmol, 33μL), PdCl 2 (MeCN) 2 (10%mmol, 1.2mg), silver fluoride (0.1mmol, 27.4mg), copper trifluoroacetate (20mmol%, 3mg), lithium fluoride (0.1mmol, 2.4mg), add dropwise 1.0mL trifluorotoluene in In a thick-walled pressure-resistant tube, tighten the stopper of the reaction tube to seal the reaction system, heat to 100°C, and react for 7 hours under the condition of stirring in an oil bath. After the reaction, the reaction solution was cooled to room temperature, filtered through short silica gel to remove insoluble impurities, washed with ethyl acetate, and the solvent was removed from the organic phase to...
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