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首页> 外文期刊>Polyhedron: The International Journal for Inorganic and Organometallic Chemistry >Synthesis, spectral characterization and crystal structure of Ni(II) pyridoxal thiosemicarbazone complexes and their recyclable catalytic application in the nitroaldol (Henry) reaction in ionic liquid media
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Synthesis, spectral characterization and crystal structure of Ni(II) pyridoxal thiosemicarbazone complexes and their recyclable catalytic application in the nitroaldol (Henry) reaction in ionic liquid media

机译：Ni（II）吡ido醛硫代半碳杂zone配合物的合成，光谱表征和晶体结构及其在离子液体介质中硝基醛（Henry）反应中的可循环催化应用

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摘要

The new square planar nickel(II) complexes 1, 2 and 3 have been synthesized from the reaction of [NiCl_2(PPh_3)_2] with the tridentate Schiff base ligand, pyridoxal thiosemicarbazone (L1), pyridoxal N-methyl thiosemicarbazone (L~2) and pyridoxal N-phenyl thiosemicarbazone (L~3) respectively in ethanol. These complexes have been characterized by elemental analyses, IR, UV-Vis, ~1H NMR, ~(31)P NMR and ESI-MS spectroscopy. The molecular structure of the complex [Ni(L~2)PPh_3] (2) was determined by single-crystal X-ray diffraction, which reveals a distorted square planar geometry around the nickel(II) ion. The nitroaldol reaction was studied in detail using the nickel(II) complexes as catalysts in a homogeneous solution formed by an ionic liquid and methanol. The effect of solvent, ionic liquid, time, temperature, catalyst loading and substituent of the ligand moiety on the reaction was also studied. The b-nitroalcohol products were obtained in good yields of up to 97%. A two step substrate addition mechanism was tentatively proposed based on ESI-MS spectral monitoring of the reaction mass.
机译：由[NiCl_2（PPh_3）_2]与三齿席夫碱配体，吡ido醛硫代半碳zone（L1），吡ido醛N-甲基硫代半碳zone（L〜2）反应合成了新的方形平面镍（II）配合物1、2和3。 ）和吡ido醛N-苯基硫代半脲（L〜3）的乙醇溶液。这些配合物已通过元素分析，IR，UV-Vis，〜1H NMR，〜（31）P NMR和ESI-MS光谱进行了表征。配合物[Ni（L〜2）PPh_3]（2）的分子结构通过单晶X射线衍射确定，揭示了镍（II）离子周围扭曲的正方形平面几何形状。在由离子液体和甲醇形成的均相溶液中，使用镍（II）配合物作为催化剂，对硝基羟醛反应进行了详细研究。还研究了溶剂，离子液体，时间，温度，催化剂负载量和配体部分的取代基对反应的影响。以高达97％的高产率获得了β-硝基醇产物。基于反应质量的ESI-MS光谱监测，初步提出了两步底物添加机理。

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