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作 者:梁现丽 温洁 陈婷 王德志 向陆军 段陆萌 杭德余 LIANG Xian-li;WEN Jie;CHEN Ting;WANG De-zhi;XIANG Lu-jun;DUAN Lu-meng;HANG De-yu(Beijing Yanhua Jilian Optoelectronic Technology Co.,Ltd.,Beijing 102502,China)
机构地区:[1]北京燕化集联光电技术有限公司,北京102502
出 处:《化学试剂》2021年第9期1309-1312,共4页Chemical Reagents
摘 要:苯并呋喃并咔唑类化合物具有卓越的给电子能力、荧光特性和结构易于修饰等优点,常被用作制备有机电致发光材料的重要中间体。使用廉价的二苯并呋喃和硼酸三异丙酯为反应物,经Suzuki-Miyaura偶联、Suzuki偶联以及Cadogan关环反应合成一种新型苯并呋喃并咔唑化合物3-溴-5H-苯并呋喃[3,2-c]咔唑,并优化合成工艺,其最佳合成工艺为:催化剂为四(三苯基膦)钯、碳酸钾提供碱性环境、邻二氯苯为Cadogan关环反应的溶剂、二氯甲烷为重结晶的溶剂。通过HPLC、^(1)HNMR和^(13)CNMR对3-溴-5H-苯并呋喃[3,2-c]咔唑的纯度和结构进行表征,并且通过DSC研究其热学性质。Benzofurocarbazole compound is used as a class of important intermediates for the preparation of organic electroluminescent materials because it owns excellent electron donating ability,fluorescence characteristic and the easy-modified structure.A simple and facile synthesis of a novel benzofurocarbazole compound 3-bromo-5H-benzofuran[3,2-c]carbazole has been achieved using low-cost dibenzofuran and triisopropyl borateas substrate by sequence of Suzuki-Miyaura coupling reaction,Suzuki coupling and Cadogan ring closure reactions.Furthermore,the synthesis process was optimized,the best process was as follows:The catalyst was tetrakis(triphenylphosphine)palladium,potassium carbonate was chosen as an alkaline,o-dichlorobenzene was the solvent for Cadogan ring closure reaction,and dichloromethane was a solvent for recrystallization.The purity and structure of 3-bromo-5Hbenzofuran[3,2-c]carbazole were characterized by HPLC,^(1)HNMR and ^(13)CNMR.Besides,its thermal property was studied by DSC.
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