2,2’,6,6’-四羧基-4,4’-联吡啶的绿色化合成  

Green Synthesis of 2,2’,6,6’-Tetracarboxy-4,4’-bipyridine

作　　者：陈地龙 刘秋华[1] 周再春[1] CHEN Di-long;LIU Qiu-hua;ZHOU Zai-chun(School of Chemistry and Chemical Engineering,Key Laboratory of Theoretical Organic Chemistry and Functional Molecules,Ministry of Education,and Hunan Provincial Key Laboratory of Controllable Preparation and Functional Application of Fine Polymers,Hunan University of Science and Technology,Xiangtan 411201,China)

机构地区：[1]湖南科技大学化学化工学院,理论有机化学与功能分子教育部重点实验室,精细聚合物可控制备及功能化应用湖南省重点实验室,湖南湘潭411201

出　　处：《精细化工中间体》2021年第3期48-51,共4页Fine Chemical Intermediates

基　　金：湖南省自然科学基金资助项目(2020JJ4292);湖南省教育厅重点项目(20A195)。

摘　　要：2,2’,6,6’-四羧基-4,4’-联吡啶是合成功能配合物和高分子材料的重要中间体。基于金属钠还原偶联,结合空气氧化方法合成了2,2’-6,6’-四甲基-4,4’-联吡啶,并用三氧化铬将其氧化成2,2’,6,6’-四羧基-4,4’-联吡啶。该方法克服了Pd催化偶联法和SO2氧化法步骤多、耗时长、污染严重的缺点,借助混合溶剂和低温相结合实现2,2’,6,6’-四羧基-4,4’-联吡啶的有效结晶,以此实现目标产品高收率的分离纯化。2,2’,6,6’-Tetracarboxy-4,4’-bipyridine is an important intermediate for the synthesis of functional complexes and polymer materials.In this work,2,2’-6,6’-tetramethyl-4,4’-bipyridine is synthesized by metal sodium reduction coupling combined with air oxidation,and chromium trioxide is used to oxidize it to obtain2,2’,6,6’-tetracarboxy-4,4’-bipyridine.This method overcomes the shortcomings of multiple steps,time-consuming,and serious pollution in the Pd catalytic coupling as well as the SO2 oxidation method;The effective crystallization of 2,2’,6,6’-tetracarboxy-4,4’-bipyridine is realized by the combination of mixed solvent and low temperature,thereby improving the separation and purification of the target product with high yield.

关 键 词：自由基反应 偶联反应 空气氧化 多功能中间体 

分 类 号：O626.2[理学—有机化学]