通过Ullmann反应合成3-吖啶酮酸  

Synthesis of 3-acridine carboxylic acid by Ullmann reaction

作　　者：申凤娟[1] 陈韶蕊[1] 

机构地区：[1]河北科技大学理学院,河北石家庄050018

出　　处：《河北工业科技》2015年第3期261-263,共3页Hebei Journal of Industrial Science and Technology

基　　金：河北省自然科学基金(B2013208016);河北省科技支撑计划项目(12213001)

摘　　要：以2-溴-1,4-二甲苯和苯胺为起始原料,通过氧化、Ullmann反应、环化生成3-吖啶酮酸。重点考察了不同溶剂、催化剂、反应时间对Ullmann反应收率的影响,确定最佳反应条件如下:以丁醇作溶剂,溴化亚铜为催化剂,于120℃加热5h得到邻苯氨基对苯二甲酸,产率为70.5%。目标化合物及中间产物的结构经核磁和质谱分析得以确证。3-acridine carboxylic acid is prepared through oxidation,Ullmann reaction,cycloisomerization from 2-bromo-p-xylene and aniline as starting material.Ullmann reaction is the key of the synthesis.Effects of the solvent,catalyst,the amount of catalyst and reaction time on the yield were investigated.The optimal reaction conditions for the Ullmann reaction are obtained as follows:Butanol is solvent,CuBr is catalyst,reaction temperature is 120℃,reaction time is 5h.Under the optimal conditions,the yield of 2-phenylamino terephthalic acid can reach 70.5%.The structure of products were characterized by 1 H NMR and MS.

关 键 词：有机合成化学 3-吖啶酮酸 ULLMANN反应 CUBR 邻苯氨基对苯二甲酸 

分 类 号：O621.3[理学—有机化学]