Multinuclear Magnetic Resonance Study on Aluminium Sec-butoxide Chelated with Ethyl Acetoacetate in Various Amounts

IF 0.7 4区 化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Croatica Chemica Acta Pub Date : 2019-09-04 DOI:10.5562/CCA3426
S. Kurajica, G. Mali, V. Mandić, I. Minga
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引用次数: 4

Abstract

Reactive aluminum alkoxide (ASB, aluminium sec-butoxide) was chelated using β-diketone (EAA, ethyl acetoacetate) in order to gain control over rapid hydrolysis in the course of the sol-gel process. Derived chelates were analysed using several NMR spectroscopic techniques: one-dimensional 1H, 13C, 27Al NMR and two-dimensional COSY, HSQC and DOSY. The NMR analysis enabled identification of the formed chelate species, as well as determination of their quantitative relationships. Several complexation products were observed: tris-chelated monomer, Al(EAA)3, bis-chelated dimmer, Al2(OnBu)4(EAA) 2, tris-chelated dimmer, Al2(OnBu)3(EAA)3, tetra-chelated dimmer, Al2(OnBu)2(EAA)4, and monochelated trimer, Al3(OnBu)8(EAA). Of the formed oligomer compounds, this is the first evidence of Al2(OR)3L3 in any alkoxide and β-ketoester or β-diketone combination. Aluminium sec-butoxide and ethyl acetoacetate complexes Al2(OnBu)4(EAA) 2 and Al2(OnBu)2(EAA)4 were also observed for the first time. With the increase of the EAA/ASB ratio the coordination of aluminium shifts towards six, whereas above the EAA/ASB ratio of 2.5 solely six-coordinated aluminium exists.
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仲丁醇铝与不同量乙酸乙酯螯合的多核磁共振研究
用β-二酮(EAA,乙乙酸乙酯)螯合活性铝醇酸盐(ASB,仲丁醇铝)以控制溶胶-凝胶过程中的快速水解。衍生的螯合物使用几种核磁共振光谱技术进行分析:一维1H, 13C, 27Al核磁共振和二维COSY, HSQC和DOSY。核磁共振分析能够识别形成的螯合物种类,以及确定它们的定量关系。观察到几种络合产物:三螯合单体Al(EAA)3,双螯合二聚体,Al2(OnBu)4(EAA) 2,三螯合二聚体,Al2(OnBu)3(EAA)3,四螯合二聚体,Al2(OnBu)2(EAA)4,单螯合三聚体Al3(OnBu)8(EAA)。在形成的低聚物化合物中,这是Al2(OR)3L3在任何醇氧化合物和β-酮酯或β-二酮组合中的第一个证据。仲丁醇铝与乙酰乙酸乙酯配合物Al2(OnBu)4(EAA) 2和Al2(OnBu)2(EAA)4也首次被观察到。随着EAA/ASB比的增加,铝的配位向6位靠拢,而在EAA/ASB比为2.5以上,铝的配位仅为6位。
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来源期刊
Croatica Chemica Acta
Croatica Chemica Acta 化学-化学综合
CiteScore
0.60
自引率
0.00%
发文量
3
审稿时长
18 months
期刊介绍: Croatica Chemica Acta (Croat. Chem. Acta, CCA), is an international journal of the Croatian Chemical Society publishing scientific articles of general interest to chemistry.
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