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Synthesis and characterization of a phosphinoferrocene ligand modified by an amidosulfonate substituent
Varmužová, Věra ; Štěpnička, Petr (advisor) ; Gyepes, Róbert (referee)
Title: Synthesis and characterization of a phosphinoferrocene ligand modified by an amidosulfonate substituent Author: Věra Varmužová Department: Department of Inorganic chemistry Supervisor: prof. RNDr. Petr Štěpnička, Ph.D., DSc. Abstract: This bachelor thesis describes the synthesis of a new compound, 1-(diphenylphosphino)-1'-(methylsulfonamino)ferrocene (compound 2), from 1,1'-dibromoferrocene. Compound 2 was prepared by reaction of 1-(diphenylphosphino)-1'-aminoferrocene-borane (1: 1) with methanesulfonyl chloride in the presence of pyridine, followed by deprotection of the diphenylphosphine group. The conditions of the reaction were optimised so that the reaction was performed with complete consamption of the starting material. The synthesis proceeds via 1-(diphenylphosphino)-1'- (methylsulfonamino)ferrocene-borane (1: 1) (compound 2), which is also a new compound. Both compounds were characterised by nuclear magnetic resonance, mass spectroscopy, infrared spectroscopy, elemental analysis and their crystal structure was determined by single- crystal X-ray crystallography. Key words: ferrocene, phosphines, sulfonamides, synthesis.
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Synthesis and coordination properties of phosphinoguanidine ligands
Leitner, Zdeněk ; Štěpnička, Petr (advisor) ; Gyepes, Róbert (referee)
Title: Synthesis and coordination properties of phosphinoguanidine ligands Author: Zdeněk Leitner Department: Department of Inorganic chemistry Supervisor: prof. RNDr. Petr Štěpnička, Ph.D. DSc. Abstract: The aim of this work was the preparation and characterisation of a hybrid P,N-donor ligand, 2-(2-(diphenylphosphanyl)phenyl)-1,3-diisopropylguanidine (compound 2), containing a polar guanidine moiety. Potential use of this ligand lies in the preparation of catalytically active complexes with a possible change of distribution between organic and water phase upon altering pH. Firstly, synthesis of the starting materiál, (2-aminophenyl)diphenylphosphine, by copper(I)- catalysed P-C coupling reaction was optimized, up to 88% yield. Preparation of compound 2 was optimized as well. Salt 4 was prepared by protonation of 2. In order to evaluate basicity of phosphine groups in the structure of 2 and 4 and an impact of guanidine moiety protonation, corresponding selenides 3 and 5 were prepared and the 1 JPSe were measured. Ligand 2 was prepared by addition of (2-aminophenyl)diphenylphosphine across 1,3-diisopropylcarbodiimide. Selenide 3 was obtained from eaction of 2 with KSeCN. Salts 4 and 5 were prepared by neutralizing compounds 2 and 3 with hydrochloric acid. All novel compounds were characterized by 1...
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Light platinum group metal complexes with a ferrocene N-phosphinoamide
Navrátil, Michal ; Štěpnička, Petr (advisor) ; Gyepes, Róbert (referee)
Title: Light platinum group metal complexes with a ferrocene N-phosphinoamide Author: Bc. Michal Navrátil Department: Department of Inorganic chemistry Supervisor: prof. RNDr. Petr Štěpnička, Ph.D., DSc. Abstract: The aim of this diploma thesis is the preparation of coordination compounds containing ferrocene phosphinoamide FcCONHPPh2 (1, Fc = ferrocenyl), whose preparation was discussed in author's bachelor thesis. Twelve new complexes are described in this thesis, including their characterisation by NMR and infrared spectroscopy, elemental analysis and mass spectrometry. In all cases the crystal structure was determined. Two palladium(II), one rhodium(III) and one ruthenium(II) precursors were used for the preparation of the complexes with each providing three new compounds. A reaction of the precursors with phosphinoamide 1 yielded complexes, in which the phosphinoamide was P-coordinated. This compound was a precursor for the other two complexes. The first one was obtained by a reaction with silver(I) perchlorate producing a cationic P,O-chelate. The other was obtained by a reaction with potassium tert-butoxide resulting in neutral P,O- chelate. All twelve complexes were prepared with optimised yields. Keywords: ferrocene, amides, phosphines, palladium, rhodium, ruthenium, structure elucidation.
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Macrocyclic complexes with open coordination sphere
Jaroš, Adam ; Kubíček, Vojtěch (advisor) ; Gyepes, Róbert (referee)
The aim of this work was to synthesize and study acid-base and coordination properties of ligands bearing a neutral or negative charge on their pendant arms. Acid-base properties of two ligands and thermodynamic stability of their complexes with gallium, copper, and zinc ions were studied using potentiometry, UV-Vis and NMR. Solid state structure of one of the ligands and its complex with copper ion was studied using RTG structural analysis. Structure of complexes in solution was studied using methods of computational chemistry.
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Synthesis and coordination properties of TACN phosphinate derivatives
Kohúteková, Soňa ; Kubíček, Vojtěch (advisor) ; Gyepes, Róbert (referee)
The aim of this work is preparation and characterization of a ligand for a selective complexation of gallium (III). The ligand is a derivative of macrocycle NOTA with bis(phosphinic) pendant arm. Protonation constants and stability constants with copper (II), nickel (II), zinc (II) and gallium (III) cations were determined by potentiometric titrations. The ligand was also used for studying complexation kinetics with gallium (III) ions and might serve as a potential contrast agent for 68 Ga-PET.
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