Unexpected simultaneous synthesis of trisubstituted quinolines and acylhydrazones under catalyst-free conditions

Trisubstituted quinolines and acylhydrazones were unexpectedly prepared from a reaction of N′-((2-aminophenyl)(phenyl)methylene)benzohydrazides with acetylenic esters. Using of N′-((2-aminophenyl)(phenyl)methylene)benzohydrazides led to obtain not only quinoline, but also a second pharmaceutical important product acylhydrazone. Notably, excellent yields, operational simplicity, short reaction times, and the avoidance of the use of catalysts make this approach an attractive complementary method to produce quinoline-2,3-dicarboxylates. The crystal structure of 5a was determined using single-crystal X-ray crystallography. The results showed that crystal packing diagram of 5a is of two pairs of molecules that have two independent alternate intermolecular 1D-polymeric H-bonds between two perpendicular molecules.     

Silica Supported Perchloric Acid:A Convenient and Environmentally Friendly Catalyst for the One-pot Multicomponent Synthesis of β-Acetamido Ketones

A modified Dakin‐West one‐pot, four‐component condensation of an aryl aldehyde, aryl ketone, acetyl chloride and acetonitrile in the presence of silica supported perchloric acid as an active, inexpensive, recoverable and recyclable catalyst is reported for the synthesis of β‐acetamido ketones under mechanical stirring and ultrasonic irradiation conditions. This system has advantages of short reaction times, good to excellent yields and the ability to carry out the large scale reactions. The use of ultrasound increases the rate of reactions compared with reactions at reflux conditions.     

Headspace solid phase microextraction of nicotine using thin layer chromatography plates modified with carbon dots

Microchimica Acta - A simple, inexpensive and efficient procedure was developed for solid-phase microextraction of nicotine from the headspace above an aqueous sample. A thin layer chromatography...     

Chromium(III) Potentiometric Sensor Based on Para‐Tertiary‐Butyl Calix[4]arene

A new chromium(III) PVC membrane sensor incorporating p‐tertiary‐butyl calix[4]arene as ionophore, potassium tetrakis as additive and dibutyl phthalate (DBP) as plasticizer was constructed. The electrode exhibited an excellent potentiometric response over a wide concentration range of 1.0×10^?7–1.0×10^?1 M with a Nernstian slope of 20±0.5 mV per decade. The detection limit was 5.0×10^?8 M. The electrode showed a better performance over a pH range of 3.0–8.0, and had a short response time of about <15 s.The electrode was successfully applied to potentiometric titration of Cr (III) with EDTA and for direct determination of chromium(III) in waste water.     

Preparation and characterization of durable micro/nanocapsules for use in self-healing anticorrosive coatings

In the field of coatings, extensive laboratory research has been conducted in the last decade. In the present work, effectiveness of epoxy resin filled micro/nanocapsules was investigated for future using in healing of cracks generated in coatings. Micro/nanocapsules were prepared by in situ polymerization of urea–formaldehyde resin to form shell over epoxy resin droplets. The optimal process parameters for synthesizing the micro/nanocapsules were selected. The as-synthesized capsules were studied by various characterizations techniques, including scanning electron microscope (SEM), particle size analyzer (PSA), Fourier transform-infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The results indicate that micro/nanocapsules containing epoxy resins can be synthesized successfully. The rough outer surface of microcapsule is composed of agglomerated urea–formaldehyde nanoparticles. They basically exhibit good storage stability at room temperature, and they are chemically stable before the heating temperature is up to approximately 250°C.     

Determination of anti‐malaria agent chloroquine using single drop liquid‐liquid‐liquid microextraction

A simple, sensitive, and inexpensive single drop liquid‐liquid‐liquid microextraction combined with isocratic RP‐HPLC and UV detection was developed for the determination of anti‐malaria drug, chloroquine. The target compound was extracted from alkaline aqueous sample solution (adjusted to 0.5 mol/L sodium hydroxide) through a thin layer of organic solvent membrane and back‐extracted to an acidic acceptor drop (adjusted to 0.02 mol/L phosphoric acid) suspended on the tip of a 25 μL HPLC syringe in the organic layer. This syringe was also used for direct injection after extraction. The linear range was 1–200 μg/L. The LOD and LOQ were 0.3 and 1.0 μg/L, respectively. Intra‐and inter‐day precisions were less than 2.0 and 2.3%, respectively. The real samples were successfully analyzed using the proposed method. The recoveries of spiked samples were more than 94.6%.     

Characteristics of the breakup and fragmentation of an electrohydrodynamic melt jet

In this study, the breakup of a melt jet into a viscous medium is investigated in the presence of an intense electric field. Fragmentation of the melt jet occurs due to both hydrodynamic and electrohydrodynamic (EHD) forces within two kinds of silicone oil of different viscosities. The size and shape characteristics of the produced particles have been studied using SEM images, and the particle size distributions were found to exhibit considerable variations when a voltage was applied and when both the viscosity and temperature of the base fluid were changed. The morphologies of the particles were also affected by the same parameters. For instance, by applying EHD force, significant enhancements in size reduction and increased roundness of the particles occurred. The breakup process of the melt jet was found to be dominant by hydrodynamic or electrohydrodynamic instabilities, depending on the situation. Governing mechanisms (instability) in the cases of pure hydrodynamic and electrohydrodynamic fragmentations are discussed.     

Chemical Composition and Antioxidant Activity of Alkanna bracteosa Essential Oil

Chemistry of Natural Compounds -     

Application of novel copper organic material for facile microextraction of sodium valproate from human plasma samples: Experimental design optimization and isotherm study

Well‐designed metal organic materials (MOMs) were synthesized and applied for pre‐concentration and determination of sodium valproate (Na‐VP) from biological samples, bound to the copper complex of 1,4‐phenylenedioxydiacetic acid under mild conditions. The channels of this sorbent provide high efficiency and also selectivity. The MOMs were structurally characterized using Fourier transform infrared and energy‐dispersive X‐ray spectroscopies, scanning electron microscopy and X‐ray diffraction, and they were found to have suitable features for quantification of Na‐VP using HPLC coupled with UV detection at λ = 215 nm. Moreover, the rate of adsorption is improved by ultrasonic power and the experimental data are best fitted according to Freundlich adsorption isotherm. According to the central composite design, the best experimental conditions are 280.0 μl, 3.0 min and 17.0 mg for volume of eluent, sonication time and sorbent mass respectively. Calibration plots show linear responses towards Na‐VP concentrations (0.4–18.0 μg ml^?1), satisfactory limit of detection (0.06 μg ml^?1, S/N = 3) and reasonable enrichment factor (70.58). The coefficient of variation values of both inter‐ and intra‐day analyses were less than 4.0%, indicating a candidate method for the determination of Na‐VP in human plasma with reasonable recovery and efficiency.