以对氯甲苯和二氯二甲基硅烷为原料,经偶联、氧化、酯化、酰肼化等系列反应,得到中间体二(4′-酰肼基苯基)-二甲基硅烷,将其与3,4,5-三辛氧基苯甲酸反应,合成了含有二甲基硅的V形二酰肼衍生物——N,N′-(4,4′-二甲基硅烷二基)双(苯甲酰基)双(3,4,5-三辛氧基苯并酰肼)。利用核磁共振氢谱仪、核磁共振碳谱仪、飞行时间质谱仪、傅里叶变换红外光谱仪对其结构进行了表征。合成的目标化合物只能在四氯化碳溶液中热可逆凝胶化,扫描电子显微镜分析表明干凝胶形貌类似火山岩结构。利用热重分析仪测定了目标化合物的热稳定性,其热分解温度为397℃,表明该化合物具有良好的热稳定性。
Using p-chlorotoluene and dichlorodimethylsilane as starting materials,a series of reactions such as coupling,oxidation,esterification and hydrazide were used to obtain the intermediate bi(4′-hydrazidediphenyl)-dimethylsilane.This was further reacted with 3,4,5-trioctyloxybenzoic acid to successfully synthesize the target compound A,a V-shaped dihydrazide derivative containing dimethyl silicon.The structure was characterized by NMR proton spectrometer,NMR carbon spectrometer,TOF-Ms(time of flight mass spectrometer) and fourier transform infrared spectroscopy.The target compound A gel factor can only be gelled thermally and reversibly in a carbon tetrachloride solution.Scanning electron microscope analysis shown that the xerogel morphology resembled volcanic rock structure.The thermal stability of the target compound A was measured by a thermogravimetric analyzer,and its thermal decomposition temperature was 397℃,indicating that the compound had good thermal stability.
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基金资助
吉林省科学技术厅重点科技研发项目(专项支持)(20180201029SF)
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