COMPLEXES OF IZOTHIADIAZOLE-CONTAINING BROMONITROSUBSTITUTED THREE UNITS PRODUCT WITH D-METALS (NI, CO, ZN)

Tatyana V. Кudayarova, M. A. Tyutina, Е. A. Danilova
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引用次数: 2

Abstract

This work is continuation of synthesis researches of substituted macroheterocyclic compounds with 1,2,4-thiadiazole fragments. Data of synthesis of complexes with divalent d-metals (Ni, Co, Zn) on the basis of received earlier brominenitrosubstituted isothiadiazole three-unit product are presented. Complexes of BAB-type product consisting 1,2,4-thiadiazole and bromine-nitro-isoindole fragments were received by interaction 3,5-bis-[5(6)-bromine-6(5)-nitro-3-iminoizoindolin-1-ilidenamiino]-1,2,4-thiadiazol with acetates of d-metals in 2-ethoxyethanol at 100 ºC for 2 h. After the reaction the mixture was poured into water and precipitate was filtered and washed with 5 % ammonia, water and hot organic solvents (acetone, methanol, dimethylformamide, pyridine). Yield of target products was 18 – 28 %. The resulting complexes are dark brown powders with high solubility in alcohols, DMF, insoluble in water, dichloromethane and hexane. The structures of products were established by data of mass spectrometry, elemental analysis, UV-vis and IR spectroscopy. Data of MALDI-TOF mass spectrometry showed that complexes with metal of three-unit product with 1,2,4-thiadiazole fragment were isolated as monohydrate by analogy with literary for 1,3,4-thiadiazole. Data of atomic absorption analysis with good convergence of the experimental and calculated values confirmed monohydrate structure these products. These complexes of three-unit products will be used for synthesis of new various substituted macroheterocycles with 1,2,4-thiadiazole fragments. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .  
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含异噻唑溴代三单位产物与d金属(ni, co, zn)的配合物
这项工作是对含1,2,4-噻二唑片段的取代大杂环化合物合成研究的延续。介绍了在已有的溴代异噻唑三元产物的基础上合成二价d-金属(Ni,Co,Zn)配合物的数据。由1,2,4-噻二唑和溴硝基异吲哚片段组成的BAB型产物的配合物通过3,5-双-[5(6)-溴-6(5)-硝基-3-亚氨基唑吲哚-1-茚二甲氨基]-1,2,4-噻二唑与d-金属在2-乙氧基乙醇中的乙酸盐在100℃下相互作用2小时而得到。反应后,将混合物倒入水中,过滤沉淀并用5%氨洗涤,水和热有机溶剂(丙酮、甲醇、二甲基甲酰胺、吡啶)。目标产品的产量为18-28%。所得络合物为深棕色粉末,在醇、DMF中具有高溶解度,不溶于水、二氯甲烷和己烷。通过质谱、元素分析、紫外-可见光谱和红外光谱等方法确定了产物的结构。MALDI-TOF质谱数据表明,1,2,4-噻二唑片段与三元产物金属的配合物是以一水合物的形式分离出来的。原子吸收分析数据与实验值和计算值具有良好的收敛性,证实了这些产物的一水合物结构。这些三个单元产物的配合物将用于合成具有1,2,4-噻二唑片段的新的各种取代的大杂环。
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CiteScore
1.40
自引率
44.40%
发文量
83
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