新型非对称二苯并[b,f][1,5]二氮杂环辛四烯的合成  

Synthesis of Novel Asymmetric Dibenzo[b,f][1,5]diazocines

作　　者：李正义[1] 李如洲 殷乐[1] 孙小强[1] LI Zheng-yi;LI Ru-zhou;YIN Yue;SUN Xiao-qiang(Jiangsu Key Laboratory of Advanced Catalytic Materials and Technology,School of Petrochemical Engineering,Changzhou University,Changzhou 213164,China)

机构地区：[1]常州大学石油化工学院江苏省绿色催化材料与技术重点实验室,江苏常州213164

出　　处：《合成化学》2020年第5期416-420,共5页Chinese Journal of Synthetic Chemistry

基　　金：国家自然科学基金资助项目(21572026);江苏省先进催化与绿色制造协同创新中心资助项目(ACGM2016-06-05)。

摘　　要：以两种不同取代的2-氨基二苯甲酮为原料,氯苯为溶剂,BF3-Et2O为脱水剂,通过分子间脱水一步环化缩合制备非对称二苯并[b,f][1,5]二氮杂环辛四烯衍生物。运用HPLC监控反应过程,优化合成工艺,得到最佳反应条件为:等物质的量的两种不同取代2-氨基二苯甲酮和BF3-Et2O,在氯苯中回流反应12 h。化合物4a^4c为新化合物,其结构经1H NMR,13C NMR和MS(ESI)表征。Using two kinds of 2-aminobenzophenones with different substituents as raw materials,chlorobenzene as solvent,BF3-Et2O as dehydrating agent,asymmetric dibenzo[b,f][1,5]diazocines were prepared by intermolecular cyclizative condensation at one step.The synthetic technology was optimized by using high performance liquid chromatography(HPLC)to monitor the reaction process.The best reaction conditions were that the equal moles of two different 2-aminobenzophenones and BF3-Et2O were reacted in refluxed chlorobenzene for 12 h.Compounds 4 a^4 c are new compounds,and their structures were characterized by 1H NMR,13C NMR and MS(ESI),respectively.

关 键 词：2-氨基二苯甲酮 二苯并[b f][1 5]二氮杂环辛四烯 非对称 合成 

分 类 号：O621.3[理学—有机化学] O626[理学—化学]