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作 者:杨振强[1] 陈鹏丽[1] 杨柳[1] 陈海涛[1] 陈辉[1] 杨瑞娜[1] YANG Zhenqiang;CHEN Pengli;YANG Liu;CHEN Haitao;CHEN Hui;YANG Ruina(Institute of Chemistry Company Limited,Henan Academy of Sciences,Zhengzhou 450002,China)
机构地区:[1]河南省科学院化学研究所有限公司,河南郑州450002
出 处:《信阳师范学院学报(自然科学版)》2019年第1期122-125,共4页Journal of Xinyang Normal University(Natural Science Edition)
基 金:国家自然科学基金项目(21502045);河南省科技创新人才计划项目(174100510018);河南省科技开放合作项目(17210600063)
摘 要:以4-溴苯腈为起始原料经过Suzuki偶联反应、Miyanra硼化反应等合成了3’-(4-溴萘-1-基)[1,1’-联苯基]-4-腈(Ⅲ),利用~1 H NMR、^(13) C NMR对其结构进行了表征.考察了反应温度、膦配体及碱等因素对3-溴-4’-腈基联苯(Ⅰ)收率的影响.结果表明,55℃为最佳反应温度、Pd_2(dba)_3作为催化剂、三(对甲苯基)膦为配体,化合物Ⅰ收率最高,达到92.3%.通过TG、荧光发射光谱研究了化合物Ⅲ的发光效率和稳定性.化合物Ⅲ具有很好的热稳定性,失重5%的温度为321.5℃.3'-(4-Bromonaphthalene-1-yl)[1,1'-biphenyl]-4-nitrile(Ⅲ) was synthesized by Suzuki reaction and Miyanra reaction using 4-bromobenzonitrile as a raw material.The structure of the compound Ⅲ was characterized by 1 H NMR and 13 C NMR.The effects of reaction temperature, alkali and phosphine ligand on the yield of the compound Ⅰ were studied.The results showed that the highest yield of the compound Ⅰwas 92.3% with Pd 2 (dba) 3 as catastyst and tri(p-tolyl)phosphine as ligand at 55 ℃ of the optimal reaction temperature.Thermal stability properties and optical properties of the compound Ⅲ were determined with TG and fluorescence spectrum.The compound Ⅲ had good thermal stability, 5% weight loss temperatures was 321.5 ℃.
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