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以亚磷酸三乙酯为偶合剂,通过偶联反应得到苯甲酸(酯)修饰的四硫富瓦烯(TTF)衍生物TTF-ph-COOCH3(7),由电子给体7水解得到含苯甲酸的电子给体TTF-ph-COOH(8)。利用1H NMR、1 3C NMR、MS等对化合物7和8进行了表征。化合物7和8的电化学性质表现出TTF体系特有的两对氧化可逆的单电子峰。同时,化合物7和8在UV-Vis光谱上都有D-A的分子内电荷转移(ICT)吸收峰,从ICT吸收的强度比较,化合物8中存在更强的D-A相互作用,即相对电子给体7,电子给体8具有更高的氧化电位相。同时,还得到了制备化合物7和8的关键中间体化合物5的单晶,并对其单晶结构进行了解析。
The triethyl phosphite is used as the coupling agent to obtain the TTF derivative TTF-ph-COOCH3 (7) modified by benzoic acid ester by the coupling reaction, which is hydrolyzed by the electron donor 7 to obtain benzene Formic acid electron donor TTF-ph-COOH (8). Compounds 7 and 8 were characterized by 1H NMR, 1 3C NMR, MS and the like. The electrochemical properties of compounds 7 and 8 exhibit two pairs of oxidatively reversible single-electron peaks peculiar to the TTF system. At the same time, both compounds 7 and 8 have intramolecular charge transfer (ICT) absorption peaks of DA in the UV-Vis spectrum. Compared with the intensity of absorption by ICT, there is a stronger DA interaction in the compound 8, that is, the relative electron donor 7 , Electron donor 8 has a higher oxidation potential phase. At the same time, the single crystal of the key intermediate compound 5 for preparing the compounds 7 and 8 was obtained, and its single crystal structure was also analyzed.