Synthesis and Ring Opening Reactions of Tetrahydroimidazo[1,5- b ][1,2,4]oxadiazol-2(1 H )-thiones

1,3-Dipolar cycloaddition of imidazoline 3-oxides 1 with methylisothiocyanate proceeds regio- and diastereoselectively to give tetrahydroimidazo[1,5- b ][1,2,4]oxadiazol-2(1 H )-thiones 3 in high yields. The cis configuration of the adducts were proved by our double cis elimination test as well as by NOESY experiments. The imidazooxadiazol-2-thiones 3a-e were treated with concentrated HCl in ethanol at 50°;C to give the corresponding 4 H -[1,2,4]oxadiazole-5-thione only in the cases where the substituent at C-6 is an aryl.     

New Heterocyclic Phosphorus Ylides: Synthesis,Crystal Structure,and Theoretical Calculation of Alkyl Substituted 3-(4-Benzoyl-1,5-diphenyl-2,3-dihydro-1H-pyrazol-3-yl)-3-oxo-2-(triphenylphosphoranylidene) Propanoates

Novel alkyl substituted 3-(4-benzoyl-1,5-diphenyl-2,3-dihydro-1H-pyrazol-3-yl)-3-oxo-2-(triphenylphosphoranylidene) propanoates (3) were synthesized from 4-benzoyl-1,5-diphenyl-1H-pyrazole-3-carbonylchloride (1) and alkyl (triphenylphosphoranylidene) acetates (2a–b). The synthesized compounds were characterized by elemental analysis, spectroscopic studies (3a–b), and single crystal X-ray diffraction (3a). The mechanism of the reaction between (1) and (2a) was studied by AM1, and the geometrical parameters of the studied molecules were also carried out in B3LYP methods with the standard 6–31G (d,p) basis set. NBO analysis were studied for 1 and 2a B3LYP methods with the standard 6–31G (d,p) basis set.     

Radioprotective and Antitumor Activity of Some Novel Amino Acids and Imidazoles Containing Thieno[2,3-d]pyrimidine Moiety

A variety of novel thieno[2,3-d]pyrimidine derivatives, comprising amino acids 3a–l, imidazothieno-pyrimidines 4A, 4b–h, and 7, were obtained via the reaction of 4-chloro-5,6-dimethylthieno[2,3-d]pyrimidine 1 with a variety of reagents. The structures of these compounds were confirmed by microanalysis, IR, ¹H NMR, and mass spectrometry. Some of the obtained compounds showed promising radioprotective and antitumor activities.     

Determination of lead separated selectively with ion exchange method from solution onto BCW in Sirnak, East Anatolia of Turkey

There are approximately 82 million of tons asphaltites reserves in ?irnak, East Anatolia of Turkey. The present study was investigated to employ ashes of S?rnak BCW (burned coal waste) as an ion exchange in removal of important toxic metal, Lead (Pb), in high yields by adsorption. The ion exchange characteristics of lead onto BCW from aqueous solution were investigated with respect to the changes in pH of solution, adsorbent dosage, initial metal ion concentration, contact time and temperature of solution. For the adsorption of lead, the Langmuir isotherm model fitted to equilibrium data better than the Freundlich isotherm model. Thermodynamic functions, the change of free energy (ΔG°), enthalpy (ΔH°) and entropy (ΔS°) of adsorption were also calculated for lead. These parameters showed that the adsorption was feasible, spontaneous and exothermic at 293–333 K. Experimental data were also evaluated in terms of kinetic characteristics of adsorption. The batch kinetic data were correlated to the pseudo-first order and pseudo-second order models. The data fitted better to the pseudo-second order equation. The activation energy of systems was determined. Experimental data have shown that BCW that was used in unmodified form; as low cost, readily available ion exchange; can be used for removal of lead from industrial waste waters. Analysis was determined using Flame Atomic Absorption Spectrometry (FAAS).     

Muscle skin temperature responses for hamstring and quadriceps to aerobic and anaerobic test conditions in Turkish Olympic Sailing Athletes

Olympic class sailing is a competitive sport and requires several abilities. An understanding of the responses to aerobic and anaerobic loading will be useful for assessing the training programs, protective strategies and possibility of injuries. Therefore, the aim of this study is to determine lower extremity main muscles skin temperature responses to aerobic and anaerobic test conditions in Turkish Olympic Sailing Athletes. Eighteen sailing athletes were assessed during preseasonal assessment period. Temperatures of quadriceps and hamstring muscle groups were evaluated bilaterally during rest and after Wingate Treadmill tests. Wingate test was accepted as an indicator of anaerobic performance and Treadmill test as an aerobic performance. Infrared thermography was performed to assess the skin temperature at anterior and posterior parts of thigh for both legs. In the triplicate comparison, the temperature changes between the rest, aerobic test and anaerobic test conditions were significant (p?<?0.05). In the analysis to determine the difference between the compared groups; for both muscle groups, temperature change after anaerobic performance was not significant; in contrast to this result the change in muscle temperature after aerobic performance was significant (p?<?0.05). Energetic—metabolic activity of major muscle groups of lower extremities during aerobic and anaerobic performance are important for injury prevention, treatment, rehabilitation and return to play. Present study shows that aerobic performance or activities requires higher energetic-metabolic activity.

     

Improved of cathode performance of LiFePO<Subscript>4</Subscript>/C composite using different carboxylic acids as carbon sources for lithium-ion batteries

Among the several materials under development for use as a cathodes in lithium-ion batteries olivine-type LiFePO₄ is one of the most promising cathode material. However, its poor conductivity and low lithium-ion diffusion limits its practical application. In this study, we report seven different carboxylic acids used to synthesize LiFePO₄/C composite, and influences of carbon sources on electrochemical performance were intensively studied. The structure and electrochemical properties of the LiFePO₄/C were characterized by X-ray diffraction, scanning electron microscopy, electrical conductivity, and galvanostatic charge–discharge measurements. Among the materials studied, the sample E with tartaric acid as carbon source exhibited the best cell performance with a maximum discharge capacity of 160 mAh g⁻¹ at a 0.1 C-rate. The improved electrochemical properties were attributed to the reduced particle size and enhanced electrical contacts by carbon.     

Polarographic and spectrophotometric determination of isocarboxazid and tranylcypromine sulphate through treatment with nitrous acid

Two methods are described for the determination of two widely prescribed antidepressants, namely isocarboxazid and tranylcypromine sulphate as the pure drugs and in dosage forms. Both methods involve prior treatment with nitrous acid. In the Spectrophotometric method, the two derivatives obey Beer's law over the concentration range 1–20 g/ml. The derivatives are polarographically reducible withE _1/2 values of –0.84 and –0.73 V for isocarboxazid and tranylcypromine sulphate, respectively. The calibration plots are linear over the range 4.3 × 10^–5–3.0 × 10^–4 and 1.1 × 10^–5–1.65 × 10^–4 mol/1 for isocarboxazid and tranylcypromine sulphate, respectively. The results obtained for assays for the two drugs compare satisfactorily with those given by the official methods.     

New conducting pyrrole–thiophene co-polymer from an oligomer precursor: electrochemical characterisation

A new oligomer of N,N′-bis(2-pyrrolyl methylene)-3,4-dicyano-2,5-diaminothiophene possessing cyano-substituted thiophene and pyrrole residues linked together by azomethine groups was used for the electrochemical polymerisation of conducting films. The approach used for the oligomer design favours inter-chain interactions through hydrogen bonding and negative charge stability through the cyano substitute thiophene. The oligomer was successfully electropolymerised at 0.67 V vs Ag⁺/Ag from 0.1M tetrabutylammonium tetrafluoroborate (TBABF₄)/acetonitrile as a dark blue film on the surface of platinum electrodes. Cyclic voltammetry has been used to investigate the redox behaviour of the films. The electrically conducting polymer showed p-doping/neutralisation behaviour. The effect of different electrolytes such as TBABF₄, tetrabutylammonium perchlorate (TBAClO₄), lithium perchlorate (LiClO₄) and sodium perchlorate (NaClO₄) on the redox switching and the stability of the polymer films was investigated. Infrared and UV-vis spectra of oligomer and polymers are presented. The evolution of the film growing process is shown by UV-vis spectroscopy.     

Fluorescent aminoarylcyclotetraphosphazenes

In the present work, octachlorocyclotetraphosphazatetraene (1), N₄P₄Cl₈, is reacted with aniline (2), 1-napthylamine (4) and 2-aminoanthracene (6) to give octakis(arylamino)cyclotetraphosphazenes (3, 5 and 7). These cyclotetraphosphazene compounds (3, 5 and 7) have been fully characterized by elemental analysis, mass (MS), FT-IR, ¹H and ³¹P NMR spectroscopies. The molecular and crystal structures of 5 have been characterized by X-ray crystallography. The structure of 5 is monoclinic with the space group P21/c. The octakis(1-napthylamino)-(5) and octakis(2-aminoanthracene)-(7) cyclotetraphosphazene compounds have been synthesised for the first time in this study. The fluorescence properties of 3, 5 and 7 have been investigated in tetrahydrofuran (THF) and have been shown to have highly fluorescence behavior. This work also presents the quenching of arylamino substituted cyclotetraphosphazene derivatives (3, 5 and 7) by p-benzoquinone (BQ) or hydroquinone (HQ).