oaioai:repozitorij.pmf.unizg.hr:pmf_7557

Sinteza i katalitička aktivnost hidrazonskih kompleksa molibdena

Abstract

As part of this diploma thesis, solution-based and mechanochemical syntheses of hydrazone compounds, obtained from 2,3-dihydroxybenzaldehyde and 2- or 4-aminobenzhydrazide (H2L1 and H2L2), was performed. Two dinuclear dioxomolybdenum(VI) complexes, [MoO2L]2, and two mononuclear complexes, [MoO2L(MeOH),] have been synthesised by the reaction of [MoO2(acac)2] and corresponding hydrazone ligand H2L in 1:1 molar ratio. Mononuclear complexes [MoO2L(MeOH)] were obtained from methanol solution, while dinuclear complexes [MoO2L]2 from acetonitrile one. Complexes were characterised by IR and NMR spectroscopies and analysed by TG and elemental analyses. The catalytic activity of all complexes was tested under organic solvent-free for the epoxidation of cis-cyclooctene and oct-1-ene with three different oxidants, aqueous tert-butyl hydroperoxide, tert-butyl hydroperoxide in decane and hydrogen peroxide, with the emphasis on the low catalyst loading (0.25 mol% vs. substrate).U sklopu ovog diplomskog rada izvedene su otopinske i mehanokemijske sinteze hidrazonskih spojeva, priređenih iz 2,3-dihidroksibenzaldehida i 2- ili 4-aminobenzhidrazida (H2L1 i H2L2). Dva dinuklearna kompleksa dioksomolibdena(VI), [MoO2L]2 i dva mononuklearna kompleksa [MoO2L(MeOH)] sintetizirani su reakcijom [MoO2(acac)2] i odgovarajućeg hidrazonskog liganda H2L u molarnom omjeru 1:1. Mononuklearni kompleksi [MoO2L(MeOH)] dobiveni su iz otopine metanola, dok dinuklearni kompleksi [MoO2L]2 iz acetonitrila. Kompleksi su karakterizirani IR i NMR spektroskopijom i analizirani TG i elementarnim analizama. Katalitička aktivnost svih kompleksa ispitana je epoksidacijom cis-ciklooktena i okt-1-ena bez dodatka organskih otapala u reakcijski medij, s tri različita oksidansa, vodenom otopinom tert-butil hidroperoksida, tert-butil hidroperoksidom u dekanu i vodikovim peroksidom, s naglaskom na mali udio katalizatora (0,25 mol.% u odnosu na supstrat)

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oaioai:repozitorij.pmf.unizg.hr:pmf_7557Last time updated on 12/29/2019

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