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Synthesis, X-ray characterization and catalytic homogenous alcohol oxidation activity of Co(II)–carboxamide complex with green oxidant (H2O2) under mild conditions
Zeitschrift für Kristallographie - Crystalline Materials ( IF 1.2 ) Pub Date : 2020-07-28 , DOI: 10.1515/zkri-2020-0038
Hakan Ünver 1
Affiliation  

Abstract In this study, a new air and moisture stable mononuclear cobalt(II)–carboxamide complex, [Co(TCrbx)2(CH3OH)2](ClO4)2, was synthesized and characterized (TCrbx = N-(4-methylpyridin-2-yl)thiophene-2-carboxamide). Complex characterization mainly was done with single crystal X-ray analysis. Ligand characterization was done with several spectroscopic techniques (Elemental Analysis, FT-IR, 1H NMR, 13C NMR). Cobalt(II) complex possesses distorted octahedral geometry coordinated with two carboxamide ligands at equatorial and two methanol ligands at axial positions and two perchlorate anions as counter ions. Synthesized complex was successfully tested as homogenous catalyst for the oxidation of benzyl alcohol with environmental friendly oxidant hydrogen peroxide (H2O2) under mild conditions. Benzaldehyde was selectively obtained with the conversion value of 99.5% in dimethyl formamide after 3-h reaction time at 50 °C with 133 TON value. Solvent and temperature effects were also investigated.

中文翻译:

Co(II)-羧酰胺配合物与绿色氧化剂 (H2O2) 在温和条件下的合成、X 射线表征和催化均相醇氧化活性

摘要 本研究合成并表征了一种新的空气和水分稳定的单核钴 (II)-甲酰胺复合物 [Co(TCrbx)2(CH3OH)2](ClO4)2 (TCrbx = N-(4-methylpyridin- 2-基)噻吩-2-甲酰胺)。复杂的表征主要是通过单晶 X 射线分析完成的。配体表征是通过几种光谱技术(元素分析、FT-IR、1H NMR、13C NMR)完成的。钴 (II) 配合物具有扭曲的八面体几何形状,与赤道的两个羧酰胺配体和轴向位置的两个甲醇配体以及两个高氯酸根阴离子作为抗衡离子相协调。合成的配合物在温和条件下作为环保型氧化剂过氧化氢 (H2O2) 氧化苯甲醇的均相催化剂成功进行了测试。在 50 °C 下反应 3 小时后,苯甲醛在二甲基甲酰胺中的转化率为 99.5%,转化率为 133 TON。还研究了溶剂和温度的影响。
更新日期:2020-07-28
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