Ruthenium(II) complexes derived from 2‐phenylthiazoline‐4‐carboxylic acid: structure and catalytic activity for transfer hydrogenation reaction

Piano‐stool ([(p‐cymene)Ru(thz)Cl], 2 ) and six‐coordinated ([Ru(thz)₂(PPh₃)₂], 3 ) ruthenium complexes derived from 2‐phenylthiazoline‐4‐carboxylic acid (Hthz, 1 ) were synthesized for the first time, and fully characterized using conventional methods. Also, the molecular structure of complex 3 was determined using X‐ray analysis. These complexes were evaluated as catalysts for transfer hydrogenation of carbonyl compounds in the presence of isopropyl alcohol and KO^tBu. Complex 2 was found to be more active than 3 in transfer hydrogenation. Copyright © 2016 John Wiley & Sons, Ltd.     

Mesoporous chitosan‐immobilized iron tetrakis(4‐carboxyphenyl)porphyrin as a model of cytochrome P‐450 enzyme for oxidation of ethylbenzene

Mesoporous chitosan‐grafted iron tetra (4‐carboxyphenyl) porphyrin catalyst (Fe TCPP/mesp‐CTS) was prepared and investigated as a practical model for the nano‐cavity and coordinate regulation‐catalysis(CRC) function in cytochrome P‐450 enzyme. Fe TCPP/mesp‐CTS was characterized by X‐ray Diffraction (XRD), Thermogravimetry (TG), Ultraviolet–visible spectroscopy(UV‐Vis), Ultraviolet–visible– Diffuse reflectance spectroscopy (UV‐DRS), Scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FT‐IR), and X‐ray photoelectron spectroscopy (XPS) techniques. The catalytic activity of Fe TCPP/mesp‐CTS for ethylbenzene oxidation was investigated and it was proved to be a better catalyst than Fe TCPP/macp‐CTS based on the ethylbenzene conversion, turnover numbers(TON), and the reusability. These results are attributed to the mesocavity and CRC of amino group in Fe TCPP/mesp‐CTS. The highest ethylbenzene conversion and yields of ketone and alcohol were 24.4% and 18.2%, respectively.     

SPE and determination by FAAS of heavy metals using a new synthesized polymer resin in various water and dried vegetables samples

Firstly, poly[phenyl thiadiazole methacrylamide-co-divinylbenzene-co-2-acrylamido-2-methylpropane sulfonic acid] (PTMAAm-co-DVB-co-AMPS), a new polymer resin was synthesized. This polymer resin was characterized by elemental analyzer, X-ray diffractometer, scanning electron microscope (SEM) and IR spectrometer. The glass column packed with the synthesized polymer resin was used for solid phase extraction (SPE). At the same time, the analytes were separated and preconcentrated from various water, dried vegetables samples and standard reference material (CRM) with SPE and determined by flame atomic absorption spectrometer (FAAS). The experimental conditions of this method such as pH, flow rates of sample, flow rates of eluent, type / concentration / volume of eluent, sample volume and matrix ions were examined. The limits of detection (µg L^?1) were calculated (3s) 0.9 for Mn(II), 1.4 for Cd(II), Co(II) and Zn(II), 1.5 for Cr(III), 2.2. for Cu(II), 1.9 for Pb(II),1.5 for Ni(II) and 1.9 for Fe(III) (n = 21). The low relative standard deviation, ≤ 2% (n = 11) and preconcentration factor as 75 for analytes were obtained.     

New chiral ruthenium(II)–phosphinite complexes containing a ferrocenyl group in enantioselective transfer hydrogenations of aromatic ketones

A new and versatile class of unsymmetrical ferrocenyl-phosphinite ligands possessing a stereogenic center has been prepared from commercially available, inexpensive aminoacids such as, d-, l-phenylglycine and d-, l-phenylalanine, through a concise synthetic procedure. These ligands are not very sensitive to air and moisture, and display good enantioselectivities in the ruthenium-catalyzed asymmetric transfer hydrogenation of acetophenone derivatives, in which up to 91% ee was obtained. A comparison of the catalytic properties of amino alcohols and other analogues based on a ferrocenyl backbone is also discussed briefly. The structures of these ligands and their corresponding complexes have been elucidated by a combination of multinuclear NMR spectroscopy, IR spectroscopy, and elemental analysis.     

On-line preconcentration and determination of Au(III) in various environmental/industrial samples by flame atomic absorption spectrometry

A rapid and simple on-line method is described for the determination of Au(III) in various samples. The method is based on the sorption of gold(III) on Lewatit MonoPlus TP207 chelating resin including the iminodiacetate group, which is used as sorbent material and packed in a minicolumn. The chemical variables such as the pH of the sample solution, eluent type, interfering ions and concentrations of reagents, and instrumental variables such as sample loading volume, reagents flow rates, and tubing length, which affect the efficiency of the method were studied and optimised. Au(III) was sorbed on the chelating resin, from which it could be eluted with 3 mol L^?1 HCl, and then introduced directly to the nebuliser-burner system of FAAS. The limit of detection of the method was 0.2 µg L^?1 while the relative standard deviation was <4.0% for 20 µg L^?1 Au(III) concentration. The preconcentration factor was found to be 106 while the optimised sample volume was 15.3 mL. The accuracy of the method was verified by analysing the certified reference material. The developed method was applied successfully for the determination of gold in different samples with satisfactory results.     

Degradation of azithromycin using Ti/RuO<Subscript>2</Subscript> anode as catalyst followed by DPV,HPLC–UV and MS analysis

The electrodegradation of azithromycin was studied by its indirect oxidation using dimensionally stable Ti/RuO₂ anode as catalyst in the electrolyte containing methanol, 0.05 M NaHCO₃, sodium chloride and deionized water. The optimal conditions for galvanostatic electrodegradation for the azithromycin concentration of 0.472 mg cm^?3 were found to be NaCl concentration of 7 mg cm^?3 and the applied current of 300 mA. The differential pulse voltammetry using glassy carbon electrode was performed for the first time in the above-mentioned content of electrolyte for the nine concentration of azithromycin (0.075–0.675 mg cm^?3) giving the limits of azithromycin detection and of quantification as: LOD 0.044 mg cm^?3 and LOQ 0.145 mg cm^?3. The calibration curve was constructed enabling the electrolyte analysis during its electrodegradation process. The electrolyte was analyzed by high-performance liquid chromatography and electrospray ionization time-of-flight mass spectrometry. The electrooxidation products were identified and after 180 min there was no azithromycin in the electrolyte while TOC analysis showed that 79% of azithromycin was mineralized. The proposed degradation scheme is presented.     

One Spot Microwave Synthesis and Characterization of Nitrogen-Doped Carbon Dots with High Oxygen Content for Fluorometric Determination of Banned Sudan II Dye in Spice Samples

Journal of Fluorescence - A simple microwave-assisted synthesis of nitrogen-doped carbon dots with high oxygen content (O-N-CDs) was carried out with citric acid as a carbon source and...