二苯并[b,f][1,2]二氮芳辛的合成研究  

Study on Synthesis of Dibenzo[b,f][1,2]Diazocine

作　　者：宋国强[1] 唐龙[1] 王羚竹[1] 王瑞瑞[1] 冯筱晴[1,2] 

机构地区：[1]常州大学制药与生命科学学院,江苏常州213164 [2]常州市药品制造与质量控制工程重点实验室,江苏常州213164

出　　处：《化学世界》2014年第1期45-49,共5页Chemical World

基　　金：江苏省普通高校研究生科研创新计划项目(CXZZ12_0730);江苏省产学研前瞻性联合研究项目(BY-2013024-20);国家级大学生创新创业训练计划项目(201310292005);江苏省高等学校大学生创新创业训练计划项目(201310292005Z)

摘　　要：以邻硝基甲苯和邻硝基苯甲醛为起始原料,在50%NaOH溶液和相转移催化剂作用下,先缩合得到2,2’-二硝基二苯乙烯,2,2’-二硝基二苯乙烯在铁粉、氯化铵、乙醇体系中还原得到2,2’-二氨基二苯乙烯,最后2,2’-二氨基二苯乙烯在无水磷酸中环合制得二苯并[b,f][1,2]二氮芳辛,并对反应条件进行了优化,总收率约为43.2%。其结构经LC-MS和1 H NMR确认。Dibenzo[b,f][1,2]diazocine was prepared from o-nitrotoluene and o-nitrobenzaldehyde through the reaction of condensation, reduction and cyclization. Firstly, 2,2＇-dinitrostilbene was obtained in 50 % sodium hydroxide solution with a phase transfer catalyst. Next, 2,2＇-diaminostilbene was synthesized from Fe/NH4Cl/EtOH system. Finally, the target compound was obtained in anhydrous phosphoric acid. The reaction conditions were optimized. The yield of the product achieved to 43.2%, and its structure was confirmed by LC-MS and 1 H NMR.

关 键 词：邻硝基甲苯 邻硝基苯甲醛 二苯并[b  f][1 2]二氮芳辛 合成 

分 类 号：O625.65[理学—有机化学]