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.
出处
《化学世界》
CAS
CSCD
北大核心
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)