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偶联法合成3,3′-联苊
Synthesis of 3,3′-Biacenaphthene by Coupling Reaction
【摘要】 为制备新型功能高分子中间体,研究了在常温常压、Lewis酸FeCl3催化下,苊的偶联反应。通过重结晶、薄层层析等方法得到了目标产物纯品,用1HNMR、FTIR和GC/MS等测试手段鉴定了其结构,表明生成的是3,3′-联苊。用GC考察了不同反应条件对3,3′-联苊产率的影响,当FeCl3和苊的摩尔比为2.3∶1.0,反应时间为5 h,溶剂为CCl4时,3,3′-联苊的产率最高。
【Abstract】 To obtain new functional aromatic polymer material,the coupling reaction of acenaphthene catalyzed by FeCl3 was investigated at ambient temperature and atmosphere.Pure 3,3′-biacenaphthenyls,which may be used as intermediate of functional aromatic polymer material,was prepared by recrystallization and chromatographic methods.The structure of 3,3′-biacenaphthenyls was identified by()1H NMR、FT IR and GC/MS analysis.The effects of various reaction conditions were studied by GC analysis.The result showed that the optimum synthesis conditions of 3,3′-biacenaphthenyls were as follows: the mole ratio of FeCl3 to acenaphthene,2.3∶1.0;the reaction time,5 h and the solvent of the reaction,CCl4.
【Key words】 Lewis acid; FeCl3; catlysis coupling reaction; 3,3′-biacenaphthenyls; intermediate;
- 【文献出处】 化学世界 ,Chemical World , 编辑部邮箱 ,2007年10期
- 【分类号】O621.3
- 【下载频次】58