Synthesis and Complexation of a Novel vic‐Dithioglyoxime

A. Cihan, S. Uysal
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Abstract

Abstract A new vic‐dioxime ligand, namely 2‐(4,5‐bishydroxyimino‐1,3‐dithiolan‐2‐ylidene)malonic acid diethyl ester (LH2), has been synthesized in two steps starting with the condensation of carbon disulphide and malonic acid diethyl ester and subsequent reaction of the dithiolate intermediate with anti‐dichloroglyoxime (DCGO) in ethanol at 5 °C. LH2 forms mononuclear N,N′‐coordinated planar metal complexes with Ni(II) and Co(II) and N,O‐coordinated (μ‐hydroxo‐bridged dimeric complex with UO2(VI). The octahedral complex (LH)2CoPyCl has been prepared by oxidation of the (LH)2Co complex in the presence of pyridine, and it has been reduced to the Co(I) derivative by NaBH4.
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一种新型vic -二硫代糖肟的合成与配位
摘要以二硫化碳与丙二酸二乙基酯缩合,二硫酯中间体与抗二氯肟(DCGO)在5℃乙醇中反应为起始步骤,合成了2 -(4,5 -双羟基亚胺- 1,3 -二硫胺- 2 -乙基)丙二酸二乙基酯(LH2)。LH2与Ni(II)和Co(II)形成单核N,N′配位的平面金属配合物,与UO2(VI)形成N,O′配位的μ羟基桥接二聚体配合物。在吡啶存在下,将(LH)2Co配合物氧化制得(LH)2CoPyCl八面体配合物,并被NaBH4还原为Co(I)衍生物。
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