62 resultados para Palladium intermediates
em Repositório Institucional UNESP - Universidade Estadual Paulista "Julio de Mesquita Filho"
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The dba-free Heck-Matsuda reaction was investigated via direct ESI-MS(/MS) monitoring. Palladium species involved in the reduction of Pd(ii) during a Wacker type reaction and several dba-free arylpalladium transient complexes were detected and characterized. Based on these findings, a more comprehensible catalytic cycle for this pivotal reaction is suggested. © 2013 The Royal Society of Chemistry.
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Chemical and structural data are reported for platinum-palladium intermediates from two nuggets found at Corrego Bom Sucesso, Minas Gerais, Brazil. Three grains with simple stoichiometries (i.e. PtxPd1 -x with x ∼0.67, ∼0.5 and ∼0.33, which correspond to Pt2Pd, PtPd and PtPd2, respectively) were characterized by single-crystal X-ray diffraction and electron-probe microanalysis. In the absence of single-crystal data it might be tempting to hypothesize that such simple stoichiometries represent distinct mineral species, however structural analyses show that all of the phases are cubic and crystallize in space group Fm3̄m. They are, therefore, natural intermediates in the palladium-platinum solid solution. Reflectance and micro-hardness values are reported for the samples and a comparison with the pure metallic elements made. On the basis of information gained from the chemical and structural characterization it can be concluded that there is a complete solid solution between Pt and Pd in nature. These findings corroborate results from experiments on synthetic compounds. © 2013 The Mineralogical Society.
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Thermal behavior of pyrazolyl complexes [PdCl2(HPz)2] (1), [PdCl2(HdmPz)2] (2), [Pd(SCN)2(HPz) 2] (3), [Pd(SCN)2(HdmPz)2] (4), [Pd(N 3)2(HdmPz)2] (5), [Pd(PzNHCO)2] (6) and [Pd(dmPzNHCO)2] (7) (HPz=pyrazole, HdmPz=3,5-dimethylpyrazole) has been studied by TG and DTA. In general, the thermal stability of [PdX 2(HL)2] (HL=HPz, HdmPz) compounds varies in the following order: HdmPz>HPz as well, according to the trends X=Cl ->SOT->NNN-. Except for 5, the [PdX 2(HL)2] complexes showed higher thermal stability than the 6 and 7 chelates. No stable intermediates were isolated during the thermal decompositions because of the overlapping degradation processes. The final products of the thermal decompositions were identified as metallic palladium by X-ray powder diffraction. © 2005 Akadémiai Kiadó, Budapest.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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The hydroalumination of butylseleno acetylenes with DIBAL-H followed by addition of n-butyllithium generated in situ the (Z)-butylseleno vinyl alanates intermediates which were captured with C(4)H(9)TeBr furnishing the (E)-telluro(seleno)ketene acetals exclusively. The isomers with opposite stereochemistry (Z)-telluro(seleno)ketene acetals were obtained by the reduction of phenylseleno acetylenes with lithium di-(isobutyl)-n-butyl aluminate hydride (Zweifel's reagent) followed by reaction of (E)-phenylseleno vinyl alanates intermediates with C(4)H(9)TeBr. (c) 2008 Elsevier Ltd. All rights reserved.
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This study describes the synthesis, IR, (1)H, and (13)C{(1)H} NMR spectroscopic as well the thermal characterization of the new palladium(II) pyrazolyl complexes [PdCl(2)(HmPz)(2)] 1, [PdBr(2)(HmPz)(2)] 2, [PdI(2)(HmPz)(2)] 3, [Pd(SCN)(2)(HmPz)(2)] 4 {HmPz = 4-methylpyrazole}. The residues of the thermal decomposition were identified as Pd(0) by X-ray powder diffraction. From the initial decomposition temperatures, the thermal stability of the complexes can be ordered in the sequence: 1 > 2 > 4 a parts per thousand 3. The cytotoxic activities of the complexes and the ligand were investigated against two murine cancer cell lines: mammary adenocarcinoma (LM3) and lung adenocarcinoma (LP07) and compared to cisplatin under the same experimental conditions.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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The pyrazole ligand 3,5-dimethyl-4-iodopyrazole (HdmIPz) has been used to obtain a series of palladium(II) complexes (1-4) of the type [PdX(2)(HdmIPz)(2)] {X = Cl(-) (1); Br(-) (2); I(-) (3); SCN(-) (4)}. All compounds have been isolated, purified, and characterized by means of elemental analysis, IR spectroscopy, (1)H and (13)C{(1)H}-NMR experiments, differential thermal analysis (DTA), and thermogravimetry (TG). The TG/DTA curves showed that the compounds released ligands in the temperature range 137-605 A degrees C, yielding metallic palladium as final residue. The complexes and the ligand together with cisplatin have been tested in vitro by MTT assay for their cytotoxicity against two murine cancer cell lines: mammary adenocarcinoma (LM3) and lung adenocarcinoma (LP07).
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Synthesis, spectroscopic characterization and thermal analysis of the compounds [Pd-2(dmba)(2)(mu-NCO)(mu-2-qnS)] (1), [Pd-2(dmba)(2)(mu-NCO)(mu-8-qnS)] (2), [Pd(2-qnS)(2)] (3) and [Pd(8-qn(S))2] (4) (dmba=N,N-dimethylbenzylamine; 2-qnS=2-quinolinethiolate; 8-qnS=8-quinolinethiolate) are described. The thermal decomposition of these compounds occurs in four consecutive steps and the final decomposition products were identified as Pd(0) by X-ray powder diffraction. The thermal stability order of the complexes is 4 > 3 > 1 > 2.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)