bis(nicotinamide) and bis(N,N-diethyl nicotinamide) p-hydroxybenzoate complexes of Ni(II), Cu(II) AND Zn(II)

The mixed-ligand p-hydroxybenzoate complexes of Ni(II), Cu(II) and Zn(II) with nicotinamide and N,N-diethylnicotinamide were synthesized and characterized by elemental analysis, magnetic susceptibility measurements and mass spectrometry. The thermal behavior of the complexes was studied by simultaneous TG, DTG and DTA methods in static air atmosphere. The infrared spectral characteristics of the complexes are also discussed. The complexes contain two water molecules, two p-hydroxybenzoato (p-hba) and two nicotinamide (na) (or diethylnicotinamide (dena)) ligands per formula unit. In these complexes, all ligands are coordinated to the metal ion as monodendate ligands. In Zn(II)-na and Cu(II)-dena complexes, thep-hydroxybenzoate behaves as bidentate chelating ligand through carboxylic oxygen atoms. The decomposition pathways and the stability of the complexes are interpreted in the terms of the structural data. The final decomposition products were found to be the respective metal oxides. This revised version was published online in July 2006 with corrections to the Cover Date.     

Furo- and thieno-fused 1,3-diazepine-4,6-diones

We report the first preparation of furo- and thieno-fused 1,3-diazepine-4,6-dione derivatives starting from ethyl 2-(2-methoxy-2-oxoethyl)-3-furancarboxylate and -thiophencarboxylate. The ester functionalities connected to the hetero-ring were converted regiospecifically into the desired amides. The ester groups attached to the methylene unit were converted into isocyanates via Curtius rearrangement. The ring-closure reaction was performed in the presence of lithium bis(trimethylsilyl)amide at room temperature to give furo- and thieno-fused diazepinone derivatives.     

Examination of performance of glassy carbon paste electrode modified with gold nanoparticle and xanthine oxidase for xanthine and hypoxanthine detection

A composite electrode was prepared by modifying glassy carbon microparticles with gold nanoparticles (Au-nps) and xanthine oxidase enzyme (XOD) for xanthine (X) and hypoxanthine (Hx) detection. After the optimization of the system for X, the biosensor was characterized for X and Hx. A linearity was obtained in the concentration range between 5.00 × 10⁻⁷ and 1.00 × 10⁻⁵ M for X with equation of y = 0.24x + 0.712 and 5.00 × 10⁻⁶ to 1.50 × 10⁻⁴ M for Hx, with equation of y = 0.014x + 0.575, respectively. Obtained results were compared to X and/or Hx biosensors including/not including Au-np in the structure. The developed system was also applied for detection of Hx in canned tuna fish sample and very promising results were obtained.     

Microencapsulated oleic–capric acid/hexadecane mixture as phase change material for thermal energy storage

Journal of Thermal Analysis and Calorimetry - Thermal energy storage systems provide efficiency in order to have better utilization of energy sources while protecting the environment. Thermal...     

Network images of drainage channels in sea spray icing by MR microscopy

An MR imaging system was developed to visualize brine drainage channels in sea spray icing. Brine pockets trapped in spray-ice matrices during ice growth are structural features of sea spray icing. Brine in the spray ice sample had drained out; therefore, using a suction pump, we filled the air gaps in the drainage channels with dodecane. In the experiments, 0.5-1.0 h was necessary to accumulate signals sufficient to obtain a 3-D micro-image; the image matrix comprised 128(3) voxels (each voxel was 200 microm per side). The MIP view showed that sea spray icing has a developed drainage-channel network structure.     

Triazine based Mn (II) and Mn (II)/Ln (III) complexes: Synthesis,characterization and catecholase activities

In the current work, two triazine‐based multidentate ligands (H₂L¹ and H₂L²) and their homo‐dinuclear Mn (II), mononuclear Ln (III) and hetero‐dinuclear Mn (II)/Ln (III) (Where Ln: Eu or La) complexes were synthesized and characterized by spectroscopic and analytical methods. Single crystals of a homo‐dinuclear Mn (II) complex {[Mn (HL¹)(CH₃OH)](ClO₄·CH₃OH}₂ ( 1 ) were obtained and the molecular structure was determined by X‐ray diffraction method. In the structure of the complex, each Mn (II) ion is seven‐coordinate and one of the phenolic oxygen bridges two Mn (II) centre forming a dimeric structure. The UV–Vis. and photoluminescence properties of synthesized ligands and their metal complexes were investigated in DMF solution and the compounds showed emission bands in the UV–Vis. region. The catecholase enzyme‐like activity of the complexes were studied for 3,5‐DTBC → 3,5‐DTBQ conversion in the presence of air oxygen. Homo‐dinuclear Mn (II) complexes ( 1 and 4 ) were found to efficiently catalyse 3,5‐DTBC → 3,5‐DTBQ conversion with the turnover numbers of 37.25 and 35.78 h^?1 (k_cat), respectively. Mononuclear Eu (III) and La (III) complexes did not show catecholase activity.     

Interactions of Imidazolium Based Ionic Liquids with Water Studied by Density and Speed of Sound Measurements: Effect of the Chain Length of an Alkyl Substituent on the Imidazolium Ion

Densities and speeds of sound of three ionic liquids (ILs), 1-ethyl-3-methyl imidazoliumtetrafluoroborate (C₂mimBF₄), 1-butyl-3-methylimidazoliumtetrafluoroborate (C₄mimBF₄) and 1-hexyl-3-methylimidazoliumtetrafluoroborate (C₆mimBF₄) were measured in aqueous solutions at (288.15, 293.15, 298.15, 303.15 and 308.15) K. These data were used to calculate the volumetric properties apparent molar volume and apparent molar isentropic compression as a function of molality. Infinite dilution values for these properties were evaluated by an extrapolation procedure based on Redlich–Meyer type equations. Apparent molar isobaric expansions at infinite dilution were also obtained from the slopes of the apparent molar volume at infinite dilution versus temperature. All these properties are interpreted in terms of IL–water interactions. The hydrolysis of the \( {\text{BF}}_{4}^{ - } \) anion of the ILs and its effects on the results is discussed.     

Synthesis of thio- and furan-fused heterocycles: furopyranone,furopyrrolone, and thienopyrrolone derivatives

We report herein the synthesis of a novel class of compounds, ethyl 4-oxo-4H-furo[3,2-c]pyran-6-yl carbonate, (7E)-7-[(dimethylamino)methylene]-4H-furo[3,2-c]pyran-4,6(7H)-dione, 5-oxo-N-phenyl-2,5-dihydro-4H-furo[3,2-b]pyrrole-4-carboxamide, and 5-oxo-N-phenyl-5,6-dihydro-4H-thieno[3,2-b]pyrrole-4-carboxamide starting from the corresponding acid derivatives. Intramolecular cyclization in the presence of thionyl chloride formed the target fused ring systems. Additional transformation was seen in the cyclization of furan-fused heterocycle. A mechanism was proposed based on experimental and computational findings.     

Diastereoselective photochromism of bisbenzothienylethenes with an oxycarbonyl-related functional group on the side chain

Nine 1-[2-(1-substituted)ethyl-3-benzothienyl]-2-(2-methyl-3-benzothienyl)hexafluorocyclopentenes (4-substituted benzoyloxy, N-arylcarbamoyloxy, and aryloxycarbonyloxy) were synthesized. They showed diastereoselective photochromic ring closure upon UV irradiation. Among them, 4-nitrophenoxycarbonyloxy-substituted compound recorded a remarkable 94% diastereomer excess with 91% conversion to the closed form.