Synthesis and biological activity of sulfur compounds showing structural analogy with combretastatin A-4

We extended our previous exploration of sulfur bridges as bioisosteric replacements for atoms forming the bridge between the aromatic rings of combretastatin A-4. Employing coupling reactions between 5-iodo-1,2,3-trimethoxybenzene and substituted thiols, followed by oxidation to sulfones with m-CPBA, different locations for attaching the sulfur atom to ring A through the synthesis of nine compounds were examined. Antitubulin activity was performed with electrophoretically homogenous bovine brain tubulin, and activity occurred with the 1,2,3-trimethoxy-4-[(4-methoxyphenyl)thio]benzene (12), while the other compounds were inactive. The compounds were also tested for leishmanicidal activity using promastigote forms of Leishmania braziliensis (MHOM/BR175/M2904), and the greatest activity was observed with 1,2,3-trimethoxy-4-(phenylthio)benzene (10) and 1,2,3-trimethoxy-4-[(4-methoxyphenyl) sulfinyl]benzene (15).

A new approach to evaluate immobilization of β-galactosidase on Eupergit® C: structural, kinetic, and thermal characterization

This study aimed to evaluate β-galactosidase immobilization. For this purpose, the ionic strength of the buffer, reaction time, amount of the immobilization support, and pH were evaluated by a central composite design. Assay 8, which consisted of 1.5 mol L-1 phosphate buffer (pH 7.5) and a reaction time of 2 h, produced the maximum yield. Eupergit® C (400 mg) was subsequently used as an immobilization support. Immobilization kinetics wereinvestigated, and a significant increase in the yield was obtained after immobilization compared with that obtained from assay 8 (22.0 U mL-1 vs. 15.6 U mL-1). The enzyme efficiency of actuation was evaluated using o-nitrophenyl-β-D-galactopyranoside and lactose, with lactose providing better results. The reuse of β-galactosidase was evaluated, and more than 50% of the initial enzyme activity was maintained after five cycles of use. Enzyme characterization revealed that immobilization improved some aspects of the thermostability of β-galactosidase.

Síntese, liofilização e caracterização de acetato de 57Fe(III)

Iron(III) acetate was synthesized by the reflux method using iron enriched in the 57Fe isotope and the compound processed by freeze-drying. The as-synthesized and freeze-dried acetates were characterized regarding their structural, thermal, vibrational and hyperfine properties. Similar diffractometric and spectroscopic results were found for both materials and also for an industrial acetate made with natural iron. However, the microstructures differed: the as-synthesized compound showed flake morphology with micrometric dimensions, whereas the freeze-dried showed flake morphology with sub-micrometric dimensions. The activation energies for thermal decomposition, calculated from the exothermic events occurring in differential scanning calorimetry measurements, were 100.9 kJ/mol (as-synthesized) and 114.7 kJ/mol (freeze-dried).

SYNTHESIS AND CHARACTERIZATION OF HDTMA-ORGANOCLAYS: INSIGHTS INTO THEIR STRUCTURAL PROPERTIES

This study aims to synthesize and characterize organoclays developed from an Argentinian montmorillonite (Bent) using hexadecyltrimethylammonium bromide (HDTMA-Br) as the intercalation agent. Subsequently, an adsorption mechanism is proposed. The obtained organoclays were more hydrophobic than the starting clay. Surfactant molecules were adsorbed initially through cation exchange in sites placed in the interlayer space of the clay. Adsorption in such sites continued until the interlayer space was saturated. Depending on the surfactant loading introduced during the intercalation process, different organizations of surfactant in the interlayer were obtained. Further adsorption of surfactant occurred in the mesopores generated by tactoids in the "house of cards" organization. This process kept surfactant molecules relatively free and out of the interlayer space.

Preparation and thermal decomposition of solid state cinnamates of alkali earth metals, except beryllium and radium

Solid state compounds of general formula ML2.nH2O [where M is Mg, Ca, Sr or Ba; L is cinnamate (C6H5 -CH=CH-COO-) and n = 2, 4, 0.8, 3 respectively], have been synthetized. Thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC) and X-ray diffraction powder patterns have been used to characterize and to study the thermal stability and thermal decomposition of these compounds.

Thermal decomposition and stability in a series of heterobimetallic carbonyl compounds of the type [Fe(CO)4(HgX)2] (X=Cl, Br, I)

Heterobimetallic carbonyl compounds of the type [Fe(CO)4(HgX)2] (X= Cl, Br, I), which have metal-metal bonds, have been prepared in order to study their thermal stabilities as a function of the halogen coordinated to mercury atoms. The characterization of the above complexes was carried out by elemental analysis, IR and NMR spectroscopies. Their thermal behaviour has been investigated and the final product was identified by IR spectroscopy and by X-ray powder diffractogram.

Structural bioinformatics study of cyclin-dependent kinases complexed with inhibitors

The present work describes molecular models for the binary complexes CDK9, CDK5 and CDK1 complexed with Flavopiridol and Roscovitine. These structural models indicate that the inhibitors strongly bind to the ATP-binding pocket of CDKs and the structural comparison with the complexes CDK2:Flavopiridol and CDK2:Roscovitine correlates the structural differences with differences in inhibition of these CDKs by the inhibitors. These structures open the possibility of testing new inhibitor families, in addition to new substituents for the already known lead structures such as flavones and adenine derivatives.

Synthesis, structural and morphological characterization of CeO2-ZnO nanosized powder systems from Pechini's method

This work reports on the investigation of nanosized CeO2-ZnO systems prepared by Pechini's method. The structural and morphological characterization of CeO2-ZnO systems as well as the characterization of CeO2 and ZnO separately, showed that the employed method result in powders with spheroidal particles whose size are in the range 30 - 200 nm, which is appropriate to provide homogeneous suspensions. The ZnO present in the prepared mixed oxides seems to increase particle size distribution and to influence the arrangement of the particles after powder dispersion.

Thermal decomposition of solid state compounds of lanthanide and yttrium benzoates in CO2 atmosphere

Solid-state Ln-Bz compounds, where Ln stands for trivalent lanthanides and Bz is benzoate have been synthesized. Simultaneous thermogravimetric and differential thermal analysis in a CO2 atmosphere were used to study the thermal decomposition of these compounds.

Analysis of the structural and electronic properties of 1-(5-Hydroxymethyl - 4 -[ 5 - (5-oxo-5-piperidin-1-yl-penta-1,3dienyl)-benzo[1,3]dioxol-2-yl] -tetrahydro-furan-2-yl)-5-methyl-1H-pyrimidine-2,4dione molecule

The structural and electronic properties of 1-(5-Hydroxymethyl - 4 -[ 5 - (5-oxo-5-piperidin- 1 -yl-penta- 1,3 -dienyl)-benzo [1,3] dioxol- 2 -yl]-tetrahydro -furan-2 -yl)-5-methy l-1Hpyrimidine-2,4dione (AHE) molecule have been investigated theoretically by performing density functional theory (DFT), and semi empirical molecular orbital calculations. The geometry of the molecule is optimized at the level of Austin Model 1 (AM1), and the electronic properties and relative energies of the molecules have been calculated by density functional theory in the ground state. The resultant dipole moment of the AHE molecule is about 2.6 and 2.3 Debyes by AM1 and DFT methods respectively, This property of AHE makes it an active molecule with its environment, that is AHE molecule may interacts with its environment strongly in solution.

Thermal stability and thermal decomposition of sucralose

Several papers have been described on the thermal stability of the sweetener, C12H19Cl3O8 (Sucralose). Nevertheless no study using thermoanalytical techniques was found in the literature. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC) and infrared spectroscopy, have been used to study the thermal stability and thermal decomposition of sweetener.

Estimation of standard enthalpy of formation of alkanes in gaseous state by calculating size, structural and electronic parameters in the molecules

A quantitative analysis is made on the correlation ship of thermodynamic property, i.e., standard enthalpy of formation (ΔH fº) with Kier's molecular connectivity index(¹Xv),vander waal's volume (Vw) electrotopological state index (E) and refractotopological state index (R) in gaseous state of alkanes. The regression analysis reveals a significant linear correlation of standard enthalpy of formation (ΔH fº) with ¹Xv, Vw, E and R. The equations obtained by regression analysis may be used to estimate standard enthalpy of formation (ΔH fº) of alkanes in gaseous state.

Decomposition of corn and soybean residues under field conditions and their role as inoculum source

Necrotrophic parasites of above-ground plant parts survive saprophytically, between growing seasons in host crop residues. In an experiment conducted under field conditions, the time required in months for corn and soybean residues to be completely decomposed was quantified. Residues were laid on the soil surface to simulate no-till farming. Crop debris of the two plant species collected on the harvesting day cut into pieces of 5.0cm-long and a 200g mass was added to nylon mesh bags. At monthly intervals, bags were taken to the laboratory for weighing. Corn residues were decomposed within 37.0 months and those of soybean, within 34.5 months. Hw main necrotrophic fungi diagnosed in the corn residues were Colletotrichum gramicola, Diplodia spp. and Gibberella zeae, and those in soybeans residues were Cercospora kikuchii, Colletotrichum spp, Glomerella sp. and Phomopsis spp. Thus, those periods shoulb be observed in crop rotation aimed at to eliminating contaminated residues and, consequently, the inoculum from the cultivated area.

Structural aspects and floristic similarity among tropical dry forest fragments with different management histories in northern Minas Gerais, Brazil

In order to produce useful knowledge to the initiatives of protection and management of forest fragments, more specifically for tropical dry forests which suffer with frequent anthropic activities, and due to the lack of specific studies, this article aimed describe the structure and the floristic similarity among three areas of dry forest with different management histories. The study was developed in Capitão Enéas municipality, Northern Minas Gerais, Brazil, where three fragments were evaluated, being one in regeneration for 30 years, another submitted to occasional fire and the third with selective cut in small scale. The sampling was developed through the point quarter method considering all the alive phanerophyte individuals with circumference at breast height (CBH) > 15 cm. In the three fragments, 512 individuals, distributed in 60 species, 47 genera, and 23 families were sampled. The most representative families were Fabaceae (26), Anacardiaceae (4), Bignoniaceae (3) and Combretaceae (3). However, fourteen families were represented by only one species. Only eight species were common to all fragments - Myracrodruon urundeuva standed out with 26.9% of all sampled individuals - while a great number of species were exclusive of each fragment. The floristic and structural differences between the fragments are possibly related to the history and intensity of management in each area besides the topography variations and the presence or absence of limestone outcrops. These results show the importance of each fragment, indicating that the loss of anyone would cause negative impacts on the regional flora and consequently to the associated biodiversity.

Litter fall production and decomposition in a fragment of secondary Atlantic Forest of São Paulo, sp, southeastern Brazil

Litter fall consists of all organic material deposited on the forest floor, being of extremely important for the structure and maintenance of the ecosystem through nutrient cycling. This study aimed to evaluate the production and decomposition of litter fall in a secondary Atlantic forest fragment of secondary Atlantic Forest, at the Guarapiranga Ecological Park, in São Paulo, SP. The litter samples were taken monthly from May 2012 to May 2013. To assess the contribution of litter fall forty collectors were installed randomly within an area of 0.5 ha. The collected material was sent to the laboratory to be dried at 65 °C for 72 hours, being subsequently separated into fractions of leaves, twigs, reproductive parts and miscellaneous, and weighed to obtain the dry biomass. Litterbags were placed and tied close to the collectors to estimate the decomposition rate in order to evaluate the loss of dry biomass at 30, 60, 90, 120 and 150 days. After collection, the material was sent to the laboratory to be dried and weighed again. Total litter fall throughout the year reached 5.7 Mg.ha-1.yr-1 and the major amount of the material was collected from September till March. Leaves had the major contribution for total litter fall (72%), followed by twigs (14%), reproductive parts (11%) and miscellaneous (3%). Reproductive parts had a peak during the wet season. Positive correlation was observed between total litter and precipitation, temperature and radiation (r = 0.66, p<0.05; r = 0.76, p<0.05; r = 0.58, p<0.05, respectively). The multiple regression showed that precipitation and radiation contributed significantly to litter fall production. Decomposition rate was in the interval expected for secondary tropical forest and was correlated to rainfall. It was concluded that this fragment of secondary forest showed a seasonality effect driven mainly by precipitation and radiation, both important components of foliage renewal for the plant community and that decomposition was in an intermediate rate.