Kinetics and related studies of the formation of 2,3‐dihydroquinazolin‐4(1H)‐ones in the presence of different benzaldehyde derivatives

The kinetics and activation parameters for the reaction between 2‐amino‐benzamide and some benzaldehyde derivatives in the presence of formic acid have been reported and discussed. A linear plot of lnk vs l/T showed that the reactions obey the Arrhenius equation. Both the Arrhenius and the Eyring equations were used to calculate the activation energy. The effect of nitro groups was studied on different positions of benzaldehyde. For all substituents, the reactions followed second‐order kinetics, and the partial orders of reactions were recognized with respect to each reactant. Comparisons between the magnitudes of ΔH^? and TΔS^?showed that the reactions were enthalpy controlled. The validity of the isokinetic relationship and the compensation effect was tested, and the isokinetic temperature (β) was obtained. A linear enthalpy‐entropy plot (ΔH^?versusΔS^?) showed that the compensation effect is established, and this process occurs via a same mechanism across a series of reactions. From the Van't Hoff and Exner's plots, the isokinetic temperature was obtained.     

An experimental investigation of substituent effects on the formation of 2,3‐dihydroquinazolin‐4(1H)‐ones: a kinetic study

The effect of different substituents on the kinetics of the reactions between 2‐amino‐benzamide and some of benzaldehyde derivatives have been spectrally investigated in the presence of formic acid. The proposed mechanism were challenged due to the determination of rate‐determining step (RDS) and also, to obtain the general rate law of the reaction. For all substituents, the reactions followed the second‐order kinetics and the partial orders of reactions were recognized with respect to each reactant. Electron withdrawing substituents on benzaldehyde ring increased the rate of reaction. Kinetic values (k and E_a) and associated activation parameters (ΔH^?, ΔG^? and ΔS^?) of the reactions were determined. Both the Arrhenius and the Eyring equations were used to calculate activation energy. Comparison of magnitude of and T showed that the reactions were enthalpy controlled. Isokinetic plots for the reactions were plotted and linear relationship between and recognized that relative contribution of enthalpy and entropy to the overall free energy was the same in the reactions.     

Substitution of poly(chlorotrifluoroethylene) with sulfur dioxide under reductive conditions

Treatment of Poly(chlorotrifluoroethylene) (in the forms of Kel-F 6061 and Neoflon M400H) with Zn/SO₂ in DMF results in substitution of the chloride ligand with the sulfinic acid moiety. Subsequent oxidation affords the sulfonic acid. The materials are characterized by elemental analysis, titration, scanning electron microscopy, and FT-IR. ATR-IR studies indicate that functionalization is probably not a surface-selective phenomenon. © 1998 John Wiley & Sons, Inc. Heteroatom Chem 9:265–269, 1998     

Electrochemical Sensing of Flutamide Contained in Plasma and Urine Matrices Using NiFe2O4/rGO Nanocomposite,as an Efficient and Selective Electrocatalyst

In this article, we report on the synthesis and new employment of magnetic nickelferrite oxide nanoparticles decorated reduced graphene oxide (NiFe₂O₄/rGO) to electrochemically sensing of flutamide. The preparation of this electrocatalyst was first assessed using various analytical instrumental techniques including FT‐IR spectroscopy, X‐ray diffraction spectroscopy, energy‐dispersive X‐ray spectroscopy, and field emission scanning and transmission electron microscopy. Besides, its electrochemical performance was investigated utilizing some electrochemical methods such as cyclic and differential pulse voltammetry, and also electrochemical impedance spectroscopy. The findings of this research are especially relevant for sensing flutamide in aqueous and biological samples. At the optimized conditions, the electrochemical sensor showed a linear range of 0.24–40.0 μmol L^?1, the detection limit of 0.05 μmol L^?1 flutamide, calibration sensitivity of 1.016 μA/μmol L^?1, and repeatability and reproducibility of 1.7 % and 4.1 %, respectively. The selectivity of the method was investigated in the presence of ions, and species can generally exist in the biological medium. The resulting data of the present work represented that this type of magnetic nanocomposites is suitable for selective detection of flutamide in real samples of plasma and urine. The recoveries obtained for flutamide analyses represented lower than 5.0 percent of relative error in these real samples.     

Well‐dispersed N‐heterocyclic carbene–palladium complex anchored onto poly(acrylic acid)/poly(vinyl alcohol) nanofibers: Novel,superior and ecofriendly nanocatalyst for the Suzuki–Miyaura cross‐coupling reaction

Polymeric nanocomposite@Pd is one of the crown jewels for the catalysis of cross‐coupling reactions. This Pd nanocomposite on various polymeric supports has been well established to catalyze cross‐coupling reactions, but its preparation supported on the surface of nanofibers has been largely overlooked. Herein, we report the preparation of a poly(acrylic acid) (PAA)/poly(vinyl alcohol) (PVA) nanofiber‐supported N‐heterocyclic carbene–Pd complex. The first step involves the preparation of PAA/PVA nanofibers using the electrospinning process. The second step comprises the reaction of water‐soluble poly(ethylene glycol)‐imidazole with modified PAA/PVA nanofibers followed by introduction of PdCl₂ to achieve successfully the desired nanocomposite. The catalytic activity of this nanocomposite was examined in the expeditious synthesis of biaryl compounds using the Suzuki–Miyaura cross‐coupling reaction under mild reaction conditions. The composite offers multiple features such as good hydrophilic properties, high surface area, admirable potential in repeatability tests and being recyclable for several runs without significant loss in its activity under the optimum reaction conditions. Our results showed the superior applicability of this novel nanocatalyst in terms of conversion reaction, yields and turnover frequencies. The structure of the catalyst was characterized using a variety of techniques.     

Quantitative Analysis of Sertraline in Human Serum by LC with Fluorescence Detection After Pre-Column Derivatization with 4-Chloro-7-nitrobenzofurazan

An accurate and sensitive reversed-phase high-performance liquid chromatographic method for analysis of sertraline in human serum, using 4-chloro-7-nitrobenzofurazan as pre-column derivatization agent, is described. The drug and an internal standard (azithromycin) were extracted from serum by use of a mixture of diethyl ether and chloroform, and subjected to pre-column derivatization with the reagent. Analysis of the resulting derivatives was performed on a 250 mm × 4.0 mm cyano column with 63:37 (v/v) methanol–sodium phosphate buffer (0.05 M, pH 3.7) containing 2 mL L^?1 triethylamine as mobile phase. Detector response was monitored at excitation and emission wavelengths of 470 and 537 nm, respectively. The calibration plot was linear over the concentration range 2–640 ng mL^?1. The lower limits of detection and quantification were 0.5 and 2 ng mL^?1, respectively. The method was validated for specificity, sensitivity, linearity, precision, accuracy, and stability and shown to be accurate (intra-day and inter-day accuracy from 0.3 to 4.2%) and precise (intra-day and inter-day precision from 2.4 to 15.5%). The drug was detected at concentrations as low as 2 ng mL^?1 in 0.5 mL serum and the method described can be easily applied to human single-dose pharmacokinetic studies of sertraline.     

One-pot synthesis of organo-silica hybrids with high thermal properties via a simple sol–gel process

Journal of Thermal Analysis and Calorimetry - Organic–inorganic hybrid composites have received much attention of scientists in the recent years due to the notable improvement of thermal...