Synthesis of 1-aryl-1-phenylpropenes using an alkylation-rearrangement-methylation-isomerization one-pot reaction sequence

(Z/E)-1-(2-Methoxyaryl)-1-phenylpropenes have been prepared in good yields by heating a mixture of a phenolic substrate, cinnamyl chloride, tetramethylammonium chloride and K₂CO3 in polyethyleneglycol at 180°C. The one-pot synthesis proceeds through four discrete reaction steps: alkylation of the phenol with cinnamyl chloride, Claisen rearrangement, O-methylation and double-bond migration. The configuration of one crystalline product was determined using a single-crystal X-ray diffraction analysis. The thermodynamic and structural features of the products were evaluated using computational chemistry techniques.      

Metathesis transformations of unsaturated derivatives of β-diketones

Selected β-diketones bearing unsaturated derivatives have been demonstrated to undergo homo-metathesis and cross-metathesis with selected olefins in the presence of Grubbs catalysts. The reactions led to respective homo- and cross-metathesis products mainly with good yields and selectivities.      

Methylcellulose/SiO<Subscript>2</Subscript> hybrids: sol-gel preparation and characterization by XRD,FTIR and AFM

Methylcellulose (MC) / SiO₂ organic / inorganic hybrid materials have been prepared from MC and methyltriethoxysilane or ethyltrimethoxysilane, and characterized by XRD, FTIR and AFM. XRD showed peak shifts. FTIR shows intermolecular hydrogen bonding between MC and SiO₂. AFM depicts surface roughness which depends on the silica precursor and MC content.      

Ceramic materials made of CdTe and Cd-Zn-Te nanocrystalline powders

In the present study newly produced semiconductor ceramic nanopowder materials made of CdTe and Cd_1−xZn_xTe (CZT) are considered. Common features and differences in microstructures, phase transformations, grain growth and properties of the ceramic materials of the binary and ternary compositions are studied.      

Structure-reactivity relationships in organosilicon chemistry revisited

Available quantitative data of the reactivity of organosilicon compounds were subjected to correlation analysis. As an alternative to the carbon chemistry values, the scale of steric constants E _S (Si) can be used for organosilicon compounds and the inductive effect is best expressed by two terms, involving the parameter of electronegativity of substituents. Alkyl substituents contribute to the reactivity exclusively through their steric effects, steric and polar effects in silicon compounds are additive and the resonance effect is insignificant. The correlation analysis can be employed in investigations of organosilicon reactions along with other methods.      

Synthesis of dibromo ketones by the reaction of the environmentally benign H<Subscript>2</Subscript>O<Subscript>2</Subscript>-HBr system with oximes

It was found that oximes undergo deoximation in the presence of the H₂O_2aq-HBr_aq system to form ketones and bromo ketones. This reaction provided the basis for the synthesis of dibromo ketones in yields varying from 40% to 94%. This method is environmentally friendly, sustainable, and easy to perform. The results of this investigation extend the potential of the use of oximes for the protection of carbonyl group, thus offering the ability to perform not only conventional deoximation but also the subsequent bromination of ketones. The reaction is easily scaled up and dibromo ketones can be prepared in gram amounts.      

Spectral study of coumarin-3-carboxylic acid interaction with human and bovine serum albumins

Fluorescence spectroscopy and circular dichroism (CD) spectroscopy were used to investigate the interaction of coumarin-3-carboxylic acid with human serum albumin (HSA) and bovine serum albumin (BSA) under physiological conditions in a buffer solution of pH 7.4.      

Calorimetric study of melts in the System KF - K<Subscript>2</Subscript>NbF<Subscript>7</Subscript>

The relative enthalpies of melts in the system KF - K₂NbF₇ were measured by drop-calorimetry at the temperatures 1058, 1140 and 1208 K as a function of composition. Heat capacities of melted mixtures and enthalpies of mixing were determined using the experimental data. The molar heat capacity of melts diverges slightly from additivity. The molar enthalpy of mixing of melts shows small negative deviation from ideality which decreases with decreasing temperature. The thermal effect at mixing was assigned predominantly to association reactions producing more complex fluoroniobate anions.      

The crystal structure of Ho<Subscript>4</Subscript>Ni<Subscript>11</Subscript>In<Subscript>20</Subscript>

The polycrystalline Ho₄Ni₁₁In₂₀ was obtained by arc-melting of the elements. The subsequent high temperature procedure was used for single crystal growth. Crystal structure of the compound was investigated by X-ray single crystal method: U₄Ni₁₁Ga₂₀ type, C 2/m, a = 22.4528(17), b = 4.2947(3), c = 16.5587(13) Å, β = 124.591(5)°, R1 = 0.0276, wR2 = 0.0493 for 1989 independent reflections with [I>2σ(I)].The structure is composed of three-dimensional network from Ni and In atoms in which Ho atoms fill distorted pentagonal channels. Open image in new window     

Total polyphenolic compounds contents (TPC), total antioxidant activities (TAA) and HPLC determination of individual polyphenolic compounds in selected Moravian and Austrian wines

Wine samples (Grüner Veltliner (GV) and Zweigelt (ZW) from four different geographical regions of Austria and Czech Republic) were analyzed to determine their total phenolic content (TPC) by applying the Folin-Ciocalteau method, total antioxidant activity (TAA) by FRAP (ferric reducing antioxidant power) and DPPH (1,1-diphenyl-2-picryl-hydrazyl) assays, and to identify and quantify eleven phenolic compounds using a HPLC/UV-VIS method.      

<Emphasis Type="Italic">N</Emphasis>-Alkylation of benzimidazoles with ketonic Mannich bases and the reduction of the resulting 1-(3-oxopropyl)benzimidazoles

Benzimidazole, benzimidazoles diversely substituted at position 2, and 5,6-dimethylbenzimidazole have been alkylated at N ¹ with ketonic Mannich bases derived from acetophenones, acetylnaphthalenes, 2-acetylthiophene and 1-tetralone to afford a series of novel 1-(3-oxopropyl)benzimidazoles. The reduction of these transamination products with NaBH₄ in methanol produced the corresponding 1-(3-hydroxypropyl)benzimidazoles in excellent yields.      

An analysis of SCF and geometry convergence for diatomic molecules

A geometry and SCF convergence study of Hartree-Fock calculations using the 6-31G* basis set is carried out on the set of all possible diatomic molecules formed from atoms with Z≤36. The utility of Hartree-Fock calculations using the smaller STO-3G basis set to improve the convergence behavior is demonstrated.      

Theoretical determination of the favorable mechanism of the reaction between AlX and HX (X = Br, Cl, and F)

The reaction mechanism between AlX and HX (X = Br, Cl, and F) have been characterized in detail using DFT as well as the ab initio method. The reaction yielding AlX₃ and molecular hydrogen was calculated to be highly exothermic. The present calculations also show that the possible routes to the trihalides species start more favorable with the primary insertion product AlX₂H than with the biadduct AlX(HX)₂ one.      

Activity and stereoselectivity of Ru-based catalyst bearing a fluorinated imidazolinium ligand

Grubbs II generation catalyst (3), bearing a fluorinated imidazolinium ligand, was investigated in cross metathesis (CM), ring closing metathesis (RCM) and ring opening polymerization metathesis (ROMP) for a variety of substrates. Kinetic studies showed reduced stability of the catalyst in methylene chloride following the first 15 minutes of reaction preventing a higher efficiency despite the very high activity. Beneficial solvent effects on the catalyst stability were observed by performing RCM in C₆F₆.      

Diironcarbonyl-coumarin complex: preparation, intramolecular electron transfer, and electro-generation of hydrogen

A new organometallic complex coupling photoactive coumarin to a diironhexacarbonyl unit has been successfully prepared and its composition and electronic structure confirmed by elemental and spectroscopic analyses. Emission spectral analysis of the complex reveals photoinduced intramolecular electron transfer from coumarin to the iron-carbonyl moiety. The compound is electrochemically reduced at −1.24 V vs. Fc/Fc⁺. This reduction is irreversible, attesting to the instability of the complex. Electrochemical evolution of hydrogen in the presence of the complex has been studied and results are discussed.      

Voltammetric determination of some alkaloids and other compounds in pharmaceuticals and urine using an electrochemically activated glassy carbon electrode

Electrochemical behaviour of some alkaloids, namely: caffeine, aminophylline, theophylline, codeine phosphate and papaverine hydrochloride, that are in solution in various combinations or in the presence of other compounds contained in pharmaceuticals or in real samples (urine) was investigated using cyclic voltammetry (CV), square-wave voltammetry (SWV) and differential pulse voltammetry (DPV) on electrochemically activated glassy carbon electrode.      

High Stokes shift long-wavelength energy gap regulated fluorescence in the series of nitro/dimethylamino-substituted ortho-analogs of POPOP

A series of novel nitro-substituted ortho-analogs of POPOP was synthesized. Like the most of the other known compounds of this class, the synthesized molecules demonstrate high Stokes shift fluorescence emission owing to the planarization of their molecules at electronic excitation. Significant fluorescence quenching in polar solvents was described as the “energy gap law” action rather than the specific effect of the dialkylamino group excited state twisting.      

Recent development in capillary ion chromatography technology

This review summarizes the development of capillary ion chromatography (CIC) over approximately the last 5 years. It mainly focuses on the technologic aspects of several key components associated with CIC, including micropump, microscale electrodialytic eluent generator, microscale suppressor and the detector.      

Synthesis,characterization and antifungal testing of 3,4-dihydropyrimidin-2(1H)-(thio)ones containing boronic acids and boronate esters

The addition of formylphenylboronic acid derivatives to thiourea and ethyl acetoacetate proceeds in the presence of an additional Lewis acid catalyst to give the corresponding 3,4-dihydropyrimidin-2(1H)-(thio)ones (Biginelli products) in moderate yield. Compounds were tested for antifungal activity against pure cultures of Aspergillus niger, Aspergillus flavus, Candida albicans and Saccharomyces cerevisiae but, unfortunately, none showed any appreciable activity.