|
|
Orgonophosphorus analogues of triphosphate
Šrein, Jakub ; Kubíček, Vojtěch (advisor) ; Štěpnička, Petr (referee)
Two substances were prepared in this work, both with PCPCP structure motif. The motif is similar to ATP molecule, although the oxygen bridges are replaced with methylene groups. Both compounds were characterized by mass spectrometry and NMR spectroscopy. Since bis(methylenephosphonato)phosphinate is soluble in water, four pKa values were determined. Both prepared compounds have potential to serve as chelating ligands. Powered by TCPDF (www.tcpdf.org)
|
|
| |
|
|
Synthesis of a ferrocenyl-substituted bicyclic phosphite
Bárta, Ondřej ; Štěpnička, Petr (advisor) ; Kubíček, Vojtěch (referee)
Title: Synthesis of a ferrocenyl-substituted bicyclic phosphite Author: Ondřej Bárta Institution: Faculty of Science, Charles University in Prague, Department of Inorganic Chemistry Supervisor: prof. RNDr. Petr Štěpnička, Ph.D. This thesis describes the synthesis of a novel bicyclic phosphite ester, {N-(2,6,7-trioxa-1-phosphabicyclo[2.2.2]oct-4-yl)carbamoyl}ferrocene (3). This compound was obtained by the reaction of phosphorus trichloride with the appropriate tris(hydroxymethyl)methyl-amide in the presence of triethylamine or pyridine. The reaction conditions were optimized by varying the solvent, reaction temperature and the base to achive the highest possible yield of the product and to enable its easy and effective chromatographic purification. A new compound, 2-ferrocenyl-4,4-bis(chloromethyl)-4,5-dihydro-1,3-oxazol (4), was isolated as the by-product of this reaction. Compound 3 was further used to prepare the carbonyl complex cis-[W(CO)4(3-κP)2] (5). All the newly prepared compounds were characterized by NMR spectroscopy, mass spectrometry, infrared spectroscopy and by elemental analysis, and their molecular structures were determined by X-ray diffraction analysis. Hydrogen bonds are cooperating to form one-dimensional chains in the crystals of phosphite 3 and solvate 4 × ½ H2O or...
|
|
|
Titania-based nanomaterials
Zabloudil, Adam ; Kubíček, Vojtěch (advisor) ; Nižňanský, Daniel (referee)
Titanium dioxide colloid with a size of particles between 20 - 40 nm was prepared. Subsequently, three substances were syntetized - methylen bis(phosphonic) acid H4L1 , 4-phosphono-butyric acid H3L2 and 4-hydroxy-4,4-diphosphono-butyric acid H5L3 . Surface of the colloidal nanoparticles was modified using these substances (H4L1 , H3L2 and H5L3 ). Then stability of these systems was studied using acid-base titration and addition of calcium ions. Keywords: TiO2, nanoparticles, surface modification
|
|
|
Synthesis and characterization of ferrocenylated amidophosphine
Horký, Filip ; Štěpnička, Petr (advisor) ; Kubíček, Vojtěch (referee)
Title: Synthesis and characterization of ferrocenylated amidophosphine. Author: Filip Horký Department: Department of Inorganic chemistry Supervisor: prof. RNDr. Petr Štěpnička, Ph.D. Abstract: Complexes with amidophosphine donors have found interesting applications in catalysis and in medicinal chemistry. This led us to synthesize {[(2-(diphenylphosphino) ethyl)]-amino]carbonyl}ferrocene (compound 1) and the corresponding phosphine oxide (compound 2). This work describes three new synthetic routes to the target amidophosphine 1. The first one is a simple reaction of ferrocenecarboxylic acid with 2-(diphenylphosphino)ethylamine with reagents mediating amide bond formation. The second approach is based on the reaction of the mentioned amine with the respective acylbenzotriazole. Finally, the third way makes use of the reaction between the amine and an active ester, pentafluorophenyl ferrocencarboxylate. All products and intermediates were characterized by NMR spectra. The newly prepared phosphine oxide 2 was further characterized by infrared spectroscopy, elemental analysis, mass spectrometry and its crystal structure was determined by single-crystal X-ray crystallography. Keywords: ferrocene ligands, ferrocene, phosphine, amide, phosphineoxide, synthesis.
|
|
|
Zirconium complexes with polyaminocarboxylate ligands
Hacaperková, Eliška ; Kubíček, Vojtěch (advisor) ; Mosinger, Jiří (referee)
This thesis is focused of zirkonium complex with polyaminocarboxylate li- gands. Formation kinetics of zirkonium complex with DTTAPPh ligand was stu- died by spectrophotometry and potentiometry with ISE electrode. According to both methods [Zr(DTTAPPh)] complex is formed rapidly (t99 % < 5 s). In the second part formation kinetics and stability of [Zr(DFO)] complex with fluo- ride anions were studied by potentiometry. For pH range 1-7 average number of fluoride anions coordinated to [Zr(DFO)] complex was determined. This de- pendence shows maxima at pH 3. Number of coordinated fluoride anions as function of increasing fluoride cincentration was studied at pH 3 and 5. Sta- bility of [Zr(DFO)(F)n] complex at fysiological pH was evaluated to determine usability of the complex in vivo.
|
|
|
Synthesis and sorption properties of bis(phosphonates)
Zabloudil, Adam ; Kubíček, Vojtěch (advisor) ; Nižňanský, Daniel (referee)
Three compounds were synthesized in this bachelor thesis- hydroxy(phenyl)methandiyl- bis(phosphonic) acid - disodium salt (Na2H2L1 ), 1-hydroxy-2-phenylethan-1,1-diyl- bis(phosphonic) acid - disodium salt (Na2H2L2 ) and tetraethyl hepta-1,6-diyne-4,4-diyl- bis(phosphonate) (L4 ). The next part of the thesis is focused on sorption towards to powdered titanium dioxide surface. Following compounds were used for these sorption experiments: Na2H2L1 , Na2H2L2 and 1-hydroxy-2-(4-nitrophenyl)ethan-1,1-diyl-bis(phosphonic) acid (H4L3 ). The experimental results show that compounds Na2H2L1 and Na2H2L2 have the ability to solubilize titanium dioxide into solution - for this reason there is no possibility to use UV-Vis spectroscopy to evaluate their sorption. In the case of H4L3 there are no solubilizing properties. The compound interacts intensively with titanium dioxide surface and forms monomolecular layer. Keywords: Bis(phosphonates), sorption, titanium dioxide.
|
|
|
Alluminium complexes for biomedical applications
Beranová, Tereza ; Kubíček, Vojtěch (advisor) ; Havlíček, David (referee)
The aim of this work was to prepare ligands of macrocycle TACN with aminophosphinate pendant arms. Two ligands were prepared and fully characterized. A complex of aluminium ion was synthesized with one of the ligand. The complex was used for studying a fluoride coordination by a fluoride ion selective electrode. Key words: macrocyclic complex, positron emission tomography, phosphinic acid
|
|
|
Synthesis of phosphinic acids
Kruliš, Tomáš ; Kubíček, Vojtěch (advisor) ; Schulz, Jiří (referee)
Two types of phosphinic acids were prepared: N,N-bis(carboxymethyl)aminomethyl phosphinic acid and carboxyethylphosphinic acid. Afterwards they were used to synthesize bisphosphinic acids: 1-hydroxy-ethan-1,1-bis[N,N-bis(carboxymethyl)aminomethyl phosphinic] acid and 1-hydroxy-ethan-1,1-bis(carboxyethyl)phosphinic acid. All compounds were characterized by NMR and mass spectroscopy. N,N-bis(carboxymethyl)aminomethylphosphinic acid was synthesized by Mannich type reaction. Carboxyethylphosphinic acid was prepared by alkylation of bis(trimethylsilyloxy)phosphine. Both bisphosphinic acids were prepared by reaction of silylesters of phosphinic acids with acetylchloride. All compounds were prepared in moderate or good yields. Keywords: Organophosphorus synthesis, phosphinic acids, bisphosphinic acids
|
|
|
Study of thermodynamic stability of complexes with polydentate ligands
Böhmová, Zuzana ; Kubíček, Vojtěch (advisor) ; Vojtíšek, Pavel (referee)
Acid-base and coordination properties of macrocyclic ligand 1-oxa-4,7- diazacyclononane-4,7-bis(methylenephosphonic acid) were investigated. Protonation constants and stability constants with Ca2+ , Mg2+ , Cu2+ , Zn2+ , Mn2+ a Ga3+ metal ions were determined by potentiometry. Keywords Potentiometry, coordination chemistry, azacycles.
|
guest ::
RSS feed.