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包含有机膦酸酯配体和金属离子的硒钨酸盐:合成、表征、磁性及在Knoevenagel缩合反应中的催化效率

Selenotungstates incorporating organophosphonate ligands and metal ions: synthesis, characterization, magnetism and catalytic efficiency in the Knoevenagel condensation reaction.

作者信息

Kong Hui, He Peipei, Yang Zongfei, Xu Qiaofei, Wang Jiawei, Ban Ran, Ma Pengtao, Wang Jingping, Niu Jingyang

机构信息

Henan Key Laboratory of Polyoxometalate Chemistry, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, Henan 475004, P. R. China.

出版信息

Dalton Trans. 2020 Jun 14;49(22):7420-7425. doi: 10.1039/d0dt00444h. Epub 2020 May 19.

DOI:10.1039/d0dt00444h
PMID:32428050
Abstract

Three sandwich-type TM-containing (TM = transition metal) organophosphonate-based polyoxotungstate clusters, [TM(HO)(SeWO){Co(OOCCHNCHPO)}] (TM = Co, Ni), have been successfully synthesized, which are the first reported TM-containing organophosphonate-based selenotungstates. They were structurally characterized by PXRD analyses, IR spectroscopy, TGA analyses, etc. Magnetic measurements show that all three compounds exhibit antiferromagnetic interactions. Besides, Co1 can be used as an efficient heterogeneous catalyst in the Knoevenagel condensation of benzaldehyde and ethyl cyanoacetate under mild conditions (60 °C), and exhibits satisfactory conversion (93%) and high selectivity (99%).

摘要

已成功合成了三种含过渡金属(TM = 过渡金属)的三明治型有机膦酸基多氧钨酸盐簇合物,即[TM(HO)(SeWO){Co(OOCCHNCHPO)}](TM = Co、Ni),它们是首次报道的含过渡金属的有机膦酸基硒钨酸盐。通过粉末X射线衍射分析、红外光谱、热重分析等手段对其结构进行了表征。磁性测量表明,这三种化合物均表现出反铁磁相互作用。此外,Co1在温和条件(60℃)下可作为苯甲醛和氰基乙酸乙酯Knoevenagel缩合反应的高效多相催化剂,转化率令人满意(93%)且选择性高(99%)。

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