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Synthesis and characterization of zeolites with controllable location of active sites
Dobiášová, Ivana ; Shamzhy, Mariya (advisor) ; Hulla, Martin (referee)
This bachelor thesis focusses on the synthesis, post-synthesis modification, and comprehensive characterization of two series of zeolites based on IWW and ITH topologies. The investigated zeolite structures were chosen because their frameworks contain d4r units preferentially occupied by Ge atoms, which can be substituted for various catalytically active metal sites such as Al, Ti, and Sn by post-synthesis degermanation/metallation. To study the influence of the chemical composition of the parent germanosilicate on the concentration and accessibility of the incorporated Al-, Ti- and Sn-associated acid sites, IWW and ITH were hydrothermally synthesized with different amounts of germanium in the reaction mixture (Si/Ge = 4 - 10 for IWW and Si/Ge = 10 - 30 for ITH) and used for post-synthesis Ge- for-metal substitution. X-ray diffraction (XRD) was used to verify the structure of the synthesized zeolites; chemical analysis identified their elemental composition; nitrogen physisorption was used to determine their textural characteristics (e.g., micropore volume, total pore volume pore, and external surface area), while scanning electron microscopy (SEM) was applied to visualize the shape and size of the zeolite particles. The coordination state of the incorporated Ti and Sn sites was studied using...
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Synthesis of ligands and reductive coupling catalysts
Žáková, Andrea ; Hulla, Martin (advisor) ; Schulz, Jiří (referee)
This thesis investigates Frustrated Lewis pair hydrogenation catalysts for the use in reductive amination reactions. A series of tin complexes using Schiff base ligands was synthetized. Their ability to act as Lewis acids in Frustrated Lewis pair catalysis was disclosed by series of experiment including Gutmann Beckett method, H2 activation using high pressure NMR measurements and hydrogenation catalytic testing. Synthetized ditriflate and monotriflate complexes were proven to reversibly activate H2 at room temperature and 60 řC respectively. All of the synthetized compounds successfully mediated imine hydrogenation confirming Frustrated Lewis pairs catalysis.
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Synthesis and characterization of bidentate P,N-donor ferrocene ligand
Rezazgui, David ; Schulz, Jiří (advisor) ; Hulla, Martin (referee)
Title: Synthesis and characterization of bidentate P,N-donor ferrocene ligand Author: Bc. David Rezazgui Department: Department of Inorganic chemistry Supervisor: RNDr. Jiří Schulz, Ph.D. The main goal of this thesis was the preparation and characterization of ferrocene ligand 4-[1'-(diphenylphosphino)ferrocen-1-yl]morpholine (compound 3). Compared to structurally similar compounds, compound 3 offers greater geometrical flexibility which might have a positive effect in some applications, for example in catalysis by transition metal complexes. Two new compounds were synthesized along the synthetic route of phosphinoamine 3, the protected amine 1 and morpholine derivate 2. Selenide 4 was prepared in order to determine the basicity of compound 3 via the direct scalar interaction of 77 Se with 31 P. The synthesis comprised phosphinylation of 1,1'-dibromoferrocene, protection of the obtained 1-bromo-1'- (diphenylphosphino)ferrocene with sulfur, azidation and immediate reduction to protected amine 1. Morpholine derivate 2 was subsequently synthesized by cyclization reaction with bis(2-chloroethyl)ether. Phosphinoamine 3 was obtained by deprotection of compound 2 with Raney nickel. Finally, selenide 4 was obtained by the reaction of 3 with KSeCN. All newly prepared compounds were analyzed by NMR and transmission...
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Synthesis and characterization of bidentate P,N-donor ferrocene ligand
Rezazgui, David ; Schulz, Jiří (advisor) ; Hulla, Martin (referee)
Title: Synthesis and characterization of bidentate P,N-donor ferrocene ligand Author: Bc. David Rezazgui Department: Department of Inorganic chemistry Supervisor: RNDr. Jiří Schulz, Ph.D. The main goal of this thesis was the preparation and characterization of ferrocene ligand 4-[1'-(diphenylphosphino)ferrocen-1-yl]morpholine (compound 3). Compared to structurally similar compounds, compound 3 offers greater geometrical flexibility which might have a positive effect in some applications, for example in catalysis by transition metal complexes. Two new compounds were synthesized along the synthetic route of phosphinoamine 3, the protected amine 1 and morpholine derivate 2. Selenide 4 was prepared in order to determine the basicity of compound 3 via the direct scalar interaction of 77 Se with 31 P. The synthesis comprised phosphinylation of 1,1'-dibromoferrocene, protection of the obtained 1-bromo-1'- (diphenylphosphino)ferrocene with sulfur, azidation and immediate reduction to protected amine 1. Morpholine derivate 2 was subsequently synthesized by cyclization reaction with bis(2-chloroethyl)ether. Phosphinoamine 3 was obtained by deprotection of compound 2 with Raney nickel. Finally, selenide 4 was obtained by the reaction of 3 with KSeCN. All newly prepared compounds were analyzed by NMR and transmission...
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