Métodos sintéticos para preparação de 2,2'-bipiridinas substituídas

The 2,2'-bipyridine has been entitled as the most widely used ligand. Nowadays there is a large variety of known molecules comprising at least two 2,2'-bipyridine units and the number of applications in many areas such as catalysis, new materials, optoeletronics and electrochemistry have increased very much in the past decades. Nevertheless, there is no article that gives an overview of the main synthetic methods for obtaining the substituted 2,2'-bipyridines, generally non available. This article presents a synthetic discussion about the three different methods (coupling reaction, ciclo-functionalization and functionalization of the heteroaromatic rings of 2,2'-bipyridine) for preparing these heterocyclic compounds and also provides a practical and fundamental guide, for obtaining more than eighty different symmetric and unsymmetrical substituted 2,2'-bipyridines, shown in a table with the corresponding references.

Química organometálica de superfície aplicada à preparação de catalisadores heterogêneos bem definidos

The study of the reactions of organometallic complexes with the surfaces of inorganic oxides, zeolites and metals constitutes the basis of Surface Organometallic Chemistry (SOMC). The basic rules of organometallic chemistry are often valid when applied to surfaces and well-defined surface organometallic complexes can be obtained. These complexes can be used as heterogeneous catalysts or, by controlled reactions, can be transformed in other species useful for a given catalytic reaction. In some cases, these catalysts exhibit higher activity and/or selectivity than their analogous molecular complexes.

Preparação de LiNbO3 e LiNbO3:Eu3+ pelo método dos precursores poliméricos

The ferroelectric compound LiNbO3 was prepared by the polymeric precursors method in the polycrystalline form containing different concentrations of Eu3+. The compounds were characterized by X-ray diffraction, vibrational and electronic spectroscopy. Electronic spectroscopy was shown to be sensitive to small concentrations of contaminating phases allowing a good control of the compound purity. The presence of Eu3+ ions leads to the formation of the LiNb3O8 phase in the range of 500 to 800 °C. Above this temperature range LiNbO3 and tetragonal (T') EuNbO4 were obtained.

Síntese e reatividade de azaindóis: aplicações na preparação de moléculas de interesse biológico

Synthetic methods used for the preparation of azaindoles are described in this article. Applications in the preparation of bioactive molecules are given: synthesis of substituted 6-azaindoles as benzodiazepines receptor ligands, substituted 7-azaindoles as dopamine D4 ligands and preparation of an olivacine analogue.

Métodos de preparação e atividade biológica do ácido quinolínico e derivados

In 1981 2,3-pyridine dicarboxylic acid (quinolinic acid) was discovery to be a selective agonist for the N-methyl -D-aspartic acid (NMDA) receptor. As a consequence it possesses neurotoxic activity resulting from overstimulation of the receptor. Quinolinic acid is implicated as an etiological factor in a range of neurodegenerative disease including AIDS related dementia, Huntington´s disease and Lyme disease. In the design of novel therapies to treat these diseases, some molecules have been identified as an important target. In this paper we described different methods to prepare quinolinic acid and derivatives.

Preparação e caracterização do complexo cobaloxima e sua utilização na construção de um eletrodo modificado: um experimento eletroquímico no curso de graduação

The present experiment describes the preparation, characterization of n-butyl(pyridil)cobaloxime complex and its electrochemical property. The infrared and uv-visible absorption spectra were used to characterize the complex obtained. The infrared spectrum of the compound showed characteristics bands that indicated the formation of the Co-C chemical bond formation. The electronic absorption spectrum in acetonitrile showed transition bands attributed to p-p*, metal-to-ligand charge transfer, d-d transitions and charge transfer Co-C. The electrochemical property was investigated by the pulse differential voltammetry technique. Two oxidation processes: Co(I)/Co(II) at -423 mV and Co(II)/Co(III) at 752 mV were observed.

Métodos de preparação de nanopartículas metálicas suportadas em carbono de alta área superficial, como eletrocatalisadores em células a combustível com membrana trocadora de prótons

Fuel cells are attracting much interest as efficient and clean energy conversion devices. The main components of low temperature fuel cells are the electrocatalysts used to promote the anodic and cathodic reactions, which are based on platinum and platinum alloys. These electrocatalysts are normally prepared in the form of metal nanoparticles supported on a conductive material, usually high surface area carbon, to improve catalyst utilization and reduce cost. This work presents and comments some methods used presently to produce these electrocatalysts. The performances of the produced electrocatalysts are compared to that of state-of-the-art commercial E-TEK electrocatalysts.

Otimização da preparação de eletrodo de pasta de carbono contendo riboflavina imobilizada em suporte inorgânico

The aim of this work was to optimize the preparation of electrodes with riboflavin (RF) immobilized on a silica surface modified with niobium oxide and carbon paste. Electrode preparation was optimized employing a factorial design consisting of two levels and three factors. The electrochemical properties of immobilized RF were investigated by cyclic voltammetry. The factorial analysis was carried out analysing the current intensity (Ipa). It was possible to optimize the electrode to get the best reversibility in the redox process, i. e. the lowest separation between anodic and cathodic peak potentials and a current ratio close to unity. The concentration of supporting electrolyte has a small effect. The proportion has the highest effect and the interaction factor between proportion and mixture has also a significant effect on the current intensity.

Influência do agente precipitante na preparação do óxido de nióbio (V) hidratado pelo método da precipitação em solução homogênea

This work reports the preparation, characterization and study of the ion exchange behavior of hydrous niobium oxide prepared by a homogeneous precipitation method. The precipitating agent was obtained in aqueous solution by thermal decomposition of urea or ammonium carbonate. The compounds were chemically and physically characterized by X-ray diffractometry, thermal analysis (TG/DTG), surface area measurements and ion exchange behavior with sodium. The materials prepared with ammonium carbonate presented a higher degree of crystallinity and better ion exchange capacity with sodium than materials prepared with urea. In the homogeneous precipitation method, materials were obtained with specific surface area of 123 - 224 m² g-1. A variation of the preparation process produced hydrous niobium oxide with a different degree of hydration and specific surface area. This provided materials with different physico-chemical properties.

Materiais híbridos orgânico-inorgânicos: preparação e algumas aplicações

The preparation and application of organic-inorganic hybrid materials are under fast development and constitute an interesting research topic on account of the versatility and wide range of applications offered by these materials. These properties can be achieved due to the mixture of the components at the molecular level. The present review covers the state of the art, the most useful preparation routes and the potential applications of these materials.

Preparação de eletrodos opticamente transparentes

A simple experiment for the preparation of transparent conducting glass electrodes by deposition of pure and fluorine doped SnO2 films is described. This procedure was tested in the undergraduate inorganic course at IQ-UNICAMP. The success in achieving a conducting layer was easily checked using the standard probes of a volt-ohm meter. The optical transmittance and thickness were studied by UV-vis spectrophotometry. To discuss the experimental results we place significant emphasis on molecular orbital and energy band model theories. The undergraduate students can also discuss the concepts related to the electronic properties of solids and to interesting new materials, such as transparent conducting films, which are the subject of significant current research and technological applications.

Preparação de compostos lamelares: síntese do hidrogenofosfato de zircônio cristalino e sua intercalação com aminas. Um experimento para estudantes de graduação

The present paper describes the synthesis of crystalline zirconium hydrogen phosphate by direct precipitation and its intercalation with pyridine and n-butylamine. The simple experiment was tested in the undergraduate inorganic chemistry laboratory course for chemistry students at IQ-UNICAMP using inexpensive reagents. The materials were characterized by powder X-ray diffraction and infrared analyses in order to obtain detailed information of the solid structure changes as a result of the intercalation process. Pyridine and n-butylamine are focused in this work as clear and elucidative examples leading to acid-base interactive processes that result in the well-formed infinite sequence of inorganic lamellar structures.

Pilarização de uma argila brasileira com poliidroxications de alumínio: preparação, caracterização e propriedades catalíticas

Montmorillonite clay from Brazil was pillared with aluminium polyhydroxications. The influence of aging of the pillaring solution and the concentration of the clay suspension on the properties of the prepared materials was studied. The materials were characterized by chemical analysis, XRD and pore analysis by N2 adsorption. The catalytic properties were evaluated in the cumene cracking reaction. Results showed that the pillarization process increases the basal spaces of natural clay from 9.7 to 18.5 Å and the surface area from 41 to 300 m²/g.

Preparação e caracterização óptica de filmes de poli(estireno sulfonados) dopados com neodímio

In this work we describe the processing of poly(styrene sulphonate) films (PSS) doped with neodymium (Nd). Optical density measurements in the UV-Vis-NIR region show the typical bands observed for neodymium chloride (NdCl3) in solution. In the case of films, the intensity ratio between the peaks at 800 nm (4I9/2 -> 4F5/2 + ²H7/2) and 580 nm (4I9/2 -> 4G5/2 + ²G7/2) is equal to 0.83. Infrared spectra present an enhancement in the absorption region of aromatic rings. Site selective luminescence spectroscopy shows that the incorporation of Nd introduces a hipsochromic shift and a line shape definition in UV luminescence compared to PSS film, decreasing the interaction between aromatic groups. In addition, the film exhibits an intense radiative transition at 1061 nm (4F3/2->4I11/2), comparable to the one present in crystalline materials doped with Nd.

Preparação e caracterização de substratos SERS ativos: um estudo da adsorção do cristal violeta sobre nanopartículas de prata

The structural characterization of molecules used in the sterilization of blood for transfusions, such as crystal violet (CV), is relevant for understanding the action of these prophylactic drugs. The characterization is feasible by surface enhanced resonance Raman spectroscopy (SERRS) of CV in solution or on surfaces. The limit of detection of CV by SERRS, in the presence of colloidal particles, using 514.5 nm as excitation radiation, was found to be around 1 ppb. The characterization of CV was also made by SERS, by using different active-particles-containing substrates, proving the versatility of this technique for the study of such structures. The results suggest that the controlled production of highly efficient SERS-active substrates may allow qualitative and quantitative analysis, with high sensitivity, with potential applications in medical and environmental fields.