Multinuclear magnetic resonance study on aluminium sec-butoxide chelated with ethyl acetoacetate in various amounts

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, 27...

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Permalink: http://skupni.nsk.hr/Record/nsk.NSK01001074251/Details
Matična publikacija: Croatica chemica acta (Online)
92 (2019), 1 ; str. 17-28
Glavni autori: Kurajica, Stanislav (Author), Gazivoda Kraljević, Tatjana, Mali, Gregor, Mandić, Vilko, Minga, Iva
Vrsta građe: e-članak
Jezik: eng
Predmet:
Online pristup: https://doi.org/10.5562/cca3426
Hrčak
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042 |a croatica 
044 |a ci  |c hr 
080 1 |a 54  |2 2011 
100 1 |a Kurajica, Stanislav  |4 aut 
245 1 0 |a Multinuclear magnetic resonance study on aluminium sec-butoxide chelated with ethyl acetoacetate in various amounts  |h [Elektronička građa] /  |c Stanislav Kurajica, Tatjana Gazivoda Kraljević, Gregor Mali, Vilko Mandić, Iva Minga. 
300 |b Graf. prikazi. 
504 |a Bibliografija: 26 jed. 
504 |a Summary. 
520 |a 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. 
653 0 |a Aluminij sec-butoksid  |a Magnetska rezonancija  |a NMR spektroskopija  |a Etil acetoacetat  |a Sol-gel postupak 
700 1 |a Gazivoda Kraljević, Tatjana  |4 aut 
700 1 |a Mali, Gregor  |4 aut 
700 1 |a Mandić, Vilko  |4 aut 
700 1 |a Minga, Iva  |4 aut 
773 0 |t Croatica chemica acta (Online)  |x 1334-417X  |g 92 (2019), 1 ; str. 17-28  |w nsk.(HR-ZaNSK)000255036 
981 |b Be2019  |b B05/19 
998 |b dalo2011 
856 4 0 |u https://doi.org/10.5562/cca3426 
856 4 0 |u https://hrcak.srce.hr/216310  |y Hrčak 
856 4 1 |y Digitalna.nsk.hr