原位还原-缩合配位法合成β-(2,4-二氨基苯氧基)乙醇-水杨醛Schiff碱锌(Ⅱ)配合物  

In Situ Preparation of β-2,4-Diaminophenoxyethanol-salicylal Schiff Base Zn(Ⅱ) Complex Compound by Reduction-condensation-complexation Method

作　　者：朱雪梅[1] 蔡照胜[1] 杨春生[1] 商士斌[2] 

机构地区：[1]盐城工学院化学与生物工程学院,江苏盐城224051 [2]中国林业科学研究院林产化学工业研究所国家林业局林产化学工程重点开放性实验室,江苏南京210042

出　　处：《化学世界》2010年第11期685-687,690,共4页Chemical World

基　　金：国家科技支撑计划资助项目(2006BAD06B10);应用化学省重点学科建设开放基金资助(XKY2009005)

摘　　要：通过原位还原-缩合配位法合成了β-(2,4-二氨基苯氧基)乙醇-水杨醛Schiff碱锌(Ⅱ)配合物,并用FTIR、1H NMR、TG-DTG和DSC方法分析了产物的结构。结果表明,在实验条件下,锌(Ⅱ)配合物的收率为53.1%,且β-(2,4-二硝基苯氧基)乙醇(2,4-DNPE)还原产物β-(2,4-二氨基苯氧基)乙醇(2,4-DAPE)的氧化被有效抑制;TG-DTG及DSC分析表明,产物在温度超过114℃时即出现明显分解,在630℃时基本分解完全;在N2氛围中,锌(Ⅱ)配合物完全分解后的残余物为原样品质量的27.81%,结合FTIR和1H NMR的分析结果,说明锌(Ⅱ)配合物为目的物。β-2,4-Diaminophenoxyethanol-salicylal Schiff base Zn（Ⅱ） complex compound（DAPE-SA Zn（Ⅱ）） was prepared by in situ reduction-condensation-complexation method.DAPE-SA Zn（Ⅱ） was characterized by FT IR,~1H NMR,TG-DTG and DSC techniques.The yield of Zn（Ⅱ） complex compound was 53.1%,and the oxidation of β-2,4-diaminophenoxyethanol（2,4-DAPE）,which was the product resulted from the reduction of β-2,4-dinitrophenoxyethanol（2,4-DNPE）,was inhibited effectively.The results of TG-DTG and DSC indicated an obvious decomposition was taken place above 114 ℃,and the decomposition reaction was completed at 630 ℃.The residual material was 27.81% when the sample was decomposed fully in the nitrogen atmosphere.Combining with the results of FT IR and ~1H NMR analysis,the product could be ascertained as DAPE-SA Zn（Ⅱ） complex compound.

关 键 词：原位还原-缩合配位 β-(2 4-二氨基苯氧基)乙醇(2 4-DAPE) β-(2 4-二硝基苯氧基)乙醇(2 4-DNPE) SCHIFF碱 

分 类 号：TQ246.31[化学工程—有机化工] O621.3[理学—有机化学]