新型双偶氮化合物的合成与表征  

Synthesis and characterization of a novel diazocompound

作　　者：刘小红[1] 林休休[1] 徐冬梅[1] 张可达[1] 

机构地区：[1]江苏省有机合成重点实验室苏州大学化学化工学院,江苏苏州215123

出　　处：《化工科技》2006年第3期23-26,共4页Science & Technology in Chemical Industry

基　　金：苏州大学在职获得博士学位人员科研资助项目(R2317224);苏州大学第四批优秀骨干教师培养人选科研资助项目(R2317144)

摘　　要：以三聚氯氰(CNC)和对羟基偶氮苯(p-HAB)为原料,通过亲核取代反应合成了一种新型双偶氮化合物。考察了反应物投料摩尔比,碱的种类和碱的用量,溶剂的种类,反应时间等条件对目标产物收率的影响。结果表明:n(p-HAB)∶n(CNC)=2∶1,碱用NaOH,且n(NaOH)∶n(CNC)=2∶1,以V(丙酮)∶V(水)=1∶1为溶剂,先在冰浴中反应2 h,再加热至30℃反应5 h,双偶氮化合物收率达94.1%。通过红外光谱,元素分析,核磁共振对目标产物结构进行了表征。A novel diazocompound was prepared from cyanuric chloride and p-hydroxyazobenzene by nucleophilic substitution reaction. The effects of the stuff molar ratio, the variety and dosage of base, the solvents, and the reaction time on the yields of the product were carefully studied. The optimum reaction condition included that the molar ratio of p-hydroxyazobenzene to cyanuric chloride was 2 ： 1, using sodium hydroxide as base and its molar ratio to cyanuric chloride was 2 ： 1 ,acetone and water as solvents and the volume ratio was 1：1, the reaction was carried out in ice bath for 2 h, then, heated to 30℃ for 5 h. In this case, the yield of the diazocompound could reach to 94.1%. The structure of the target product was characterized by elementary analysis, IR spectrum and IH-NMR.

关 键 词：双偶氮化合物 对羟基偶氮苯 三聚氯氰 

分 类 号：TQ246.5[化学工程—有机化工]