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Doctoral Thesis
DOI
10.11606/T.75.2012.tde-05072012-083858
Document
Author
Full name
André Gustavo de Araujo Fernandes
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Carlos, 2012
Supervisor
Committee
Deflon, Victor Marcelo (President)
Frem, Regina Célia Galvao
Lima Neto, Benedito dos Santos
Ferreira, Ana Maria da Costa
Marques, Fabio Luiz Navarro
Title in Portuguese
Quelato-complexos de rênio e tecnécio com potencial aplicação medicinal
Keywords in Portuguese
Medicina
Rênio
Tecnécio
Abstract in Portuguese
Neste trabalho foram estudadas as formas de coordenação de piridinonas, ditiocarbazatos e N-(N'',N''-dialquilaminotiocarbonil)-N'-(2-hidroxifenil)benzoamidinas aos centros metálicos Re (V) e Tc (V). Neste sentido, os complexos triclorobis(trifenilfosfina)oxorrênio(V), [ReOCl3(PPh3)2]57, tribromobis(trifenilfosfina)oxorrênio(V), [ReOBr3(PPh3)2]57, e tetraclorooxorenato(V) de tetrabutilamônio, (NBu4)[ReOCl4]58, foram sintetizados e utilizados como precursores. O precursor tetraclorooxotecnetato(V) de tetrabutilamônio, (NBu4)[TcOCl4], foi sintetizado e disponibilizado pelo grupo de Prof. Dr. Ulrich Abram, da Universidade Livre de Berlin, durante o período de trabalho realizado na Alemanha.
Foram utilizadas as seguintes técnicas para a caracterização dos complexos sintetizados: espectroscopia de absorção na região do infravermelho, análise elementar (C, H, N e S), espectroscopia de ressonância magnética nuclear (31P, 1H e no caso de um dos complexos, também 13C), espectrometria de massas (MS-ESI) e determinação de estruturas cristalinas e moleculares, quando possível, por difração de raios X em monocristal. Por se tratar de um elemento radioativo, a avaliação do percentual de tecnécio em seus complexos foi determinada por meio da técnica de cintilação líquida.
Deste o início deste trabalho foram sintetizados e caracterizados por diversas técnicas 14 novos complexos de rênio e 1 de tecnécio, todos inéditos. Seis ditiocarbazatos, sendo 5 inéditos, também foram sintetizados e caracterizados.
Title in English
Rhenium and technetium chelate-complexes of potential medicinal application
Keywords in English
Medicine
Rhenium
Technetium
Abstract in English
This work evaluated the coordination mode of pyridinones, dithiocarbazates and N-(N'',N''-Diethylaminothiocarbonyl)-N'-(2-hydroxyphenyl)benzamidine, to the metal centers Re (V) and Tc (V). For this purpose, the compounds trichlorobis(triphenylphosphine)oxorhenium(V), [ReOCl3(PPh3)2]43, tribromobis(triphenylphosphine)oxorhenium(V), [ReOBr3(PPh3)2]43, and tetra-n-butyl)ammonium tetrachlorooxorhenate(V), (NBu4)[ReOCl4]44, were synthesized and used as starting materials. The precursor tetra-n-butylammonium tetrachlorooxotechnetate(V), (NBu4)[TcOCl4] was synthesized and released by the Prof. Dr. Ulrich Abram's group, at the Freie Universität Berlin, during my research time in Germany.
The complexes were characterized by infrared absorption spectroscopy, elemental analyses (CHNS), mass spectrometry with electrospray ionization (MSESI), nuclear magnetic resonance spectroscopy (31P, 1H and, in one case, also 13C) and had their crystalline and molecular structures, when possible, properties determined by X-ray diffraction on single crystals. Due to its radioactive element, the 99Tc values were determined by standard liquid scintillation counting.
Since the beginning of this work were synthesized and characterized by various techniques 14 new rhenium and 1 technetium complexes, all of then unknown in the literature. All the complexes presented here were obtained in good or excellent yields. Six new dithiocarbazates were obtained and characterized, of which 5 are unknown.
 
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Publishing Date
2012-07-31
 
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