N,N′-双(3-甲基苯基)-N,N′-二苯基联苯胺的合成  

Synthesis of N,N′-Dipheny-N,N′-bis(3-methylphenyl)benzidine

作　　者：聂海[1] 唐先忠[1] 李元勋[1] 

机构地区：[1]电子科技大学微电子与固体电子学院应用化学系,四川成都610054

出　　处：《精细化工》2003年第9期522-523,531,共3页Fine Chemicals

摘　　要：以二苯胺为起始原料,经两步反应合成了有机电致发光材料N,N′ 双(3 甲基苯基) N,N′ 二苯基联苯胺(TPD)。通过优化实验得到最佳的合成工艺为:二苯胺在20℃下,以V(冰醋酸)∶V(水)=1∶4为溶剂,加入重铬酸钾进行反应得N,N′ 二苯基联苯胺,分离提纯后,再加入18 冠 6相转移催化剂,以邻二氯苯为溶剂在氮气保护下与间碘甲苯进行乌尔曼反应,在200℃下反应20h,产物经柱层析和重结晶提纯。TPD收率为85%,较文献提高5%,w(TPD)=99 92%。并用元素分析、红外光谱和核磁共振对产物的结构进行了表征。N,N′DiphenyN,N′bis(3methylphenyl)benzidine (TPD) for organic electroluminescent material was synthesized using diphenylamine as starting material through two step reactions.Thus,as optimized technology,N,N′diphenylbenzidine(Ⅰ) was prepared through the reaction of diphenylamine with potassium dichromate at 20 ℃,using V(HAC)∶V(H2O)=1∶4 as solvent,and then Ullmann reaction was progressed with Ⅰ and miodotoluene under the protection of N2 at 200 ℃ for 20 h,adding 18crown6 as phase transfer catalyst and odichlorobenzene as solvent.The product was purified by column chromatography and recrystallization.TPD was obtained in 85% yield,which was 5% higher than that reported in literature.The purity of TPD was 9992% and its structure was characterized by elementary analysis,IR and NMR.

关 键 词：有机电致发光材料 N N’-双(3-甲基苯基)-N N’-二苯基联苯胺 乌尔曼反应 

分 类 号：TQ246.3[化学工程—有机化工]