摘要
以3-羧基水杨醛与二氨基硫脲为原料，在酸性条件下，以甲醇为溶剂，合成了3-羧基水杨醛双缩二氨基硫脲席夫碱（H2L）及其单核配合物NiL和异双核配合物NiML（M=Mn^3＋，Fe^3＋，Co^2＋，Cu^2＋，Zn^2＋）。考察了反应时间、温度、原料配比对该合成的影响。结果表明，反应的最佳条件为：3-羧基水杨醛：二氨基硫脲=2．4：1（摩尔比），在70—80℃条件下反应3h，产率可达78％。通过元素分析、^1HNMR、IR、UV-vis、摩尔电导等手段对合成得到的席夫碱化合物的组成和结构进行表征。
The Schiff base ligand（H2L） and its mononuclear complex NiL and heterobinuclear complexes NiML （M=Mn^3＋,Fe^3＋,Co^2＋,Cu^2＋,Zn^2＋） have been synthesized by the reaction of 3-carboxylsalicyl- aldehyde,dithio-carbohydrazon as main materials and under the condition of acid and methanol as solvent. After testing the effect of mixture ratio, reaction temperature and time on reaction carefully. The result shows that the optimum condition as follows：the mole ratio of 3-carboxylsalicylaldehyde to dithiocar-bohydrazon is 2.4 ： 1, the reaction time is 3 h at condition of 70 - 80 ℃. The production rate can amount to 78%. The H2L and its complexes have been characterized by elemental analysis,^1H NMR,IR and UV spectra and molar conductance.
出处
《应用化工》
CAS
CSCD
2008年第7期790-793,共4页
Applied Chemical Industry
关键词
二氨基硫脲
席夫碱配合物
合成
表征
dithio carbohydrazon
Schiff base
synthesis
characterization
