Preparation and characterization of new inorganic–organic hybrid catalyst H3PMo12O40/Hyd‐SBA‐15 and its application in the domino multi‐component reaction

We present novel inorganic–organic hybrid catalyst to accomplish domino multi‐component reaction (MCR) for synthesis of 3‐amino‐2′‐oxospiro[benzo[c]pyrano[3,2‐a]phenazine‐1,3′‐indoline]‐2‐carbonitrile/carboxylate derivatives. This methodology offers remarkable development by easy production of H₃PMo₁₂O₄₀/Hyd‐SBA‐15 in regard to solving the problem of using harsh catalysts, also it demonstrates to be impressive and environmentally friendly in term of low reaction times and high yields.     

Synergetic catalytic effect of rGO,Pd, Fe3O4 and PPy as a magnetically separable and recyclable nanocomposite for coupling reactions in green media

In this paper, rGO/Pd–Fe₃O₄@PPy as an efficient stable nanocomposite was synthesized. To understand the synergetic effects of rGO, Pd, Fe₃O₄ and PolyPyrrole, the performance of rGO/Pd–Fe₃O₄@PPy as a heterogeneous recyclable nanocatalyst in the green synthesis of C‐C and C‐O coupling products, as well as different conditions are studied. Synthesized rGO/Pd–Fe₃O₄@PPy was characterized by FT‐IR, XRD, FE‐SEM, EDS, TGA and AFM analysis. Best results are obtained under sonication in H₂O for C‐C coupling and by ball‐milling for C‐O coupling. The benefits of this method include: green solvents and conditions, absence of external base, low reaction times with high yield and easy work‐up method.     

Determination of cetirizine and its impurities in bulk and tablet formulation using a validated capillary zone electrophoretic method

A stability indicating capillary electrophoretic method for separation and determination of cetirizine dihydrochloride and its major impurities in bulk and a tablet dosage form was developed. The electrophoretic separation was performed in an uncoated fused-silica capillary (75 cm × 50 μm i.d.) using 75 mM sodium phosphate (pH 2.8) as background electrolyte, with an applied voltage of +25 kV at 25°C and UV detection at 230 nm. Fexofenadine was used as internal standard. The proposed method was found selective for determination of the main drug and its major impurities. The regression data obtained from the calibration plots indicated linear relationship (r ² = 0.998) over the concentration range of 40–240 μg/mL of cetirizine. Repeatability and reproducibility of the method, assessed as intra-day and inter-day variation and expressed as RSD (%), were 1.3 and 2.6, respectively. Stress tests on cetirizine under acidic, basic, oxidative and heat incubating at 80°C conditions revealed that no major compound was formed under the applied conditions and the proposed CE method is applicable for stability studies on cetirizine. Then, the method was successfully applied to the determination of cetirizine in bulk and a tablet dosage form.     

Determination of lithium isotopic composition by thermal ionization mass spectrometry in seawater

The isotopic composition of lithium in seawater has been determined by thermal ionization mass spectrometry (TIMS) based on the use of lithium hydroxide as the ion source. Isotopic measurements in a reference material supplied by IAEA (L-SVEC Li₂CO₃) were made to check the reproducibility of the method and ⁶Li indicates mobilization of light isotope of lithium form the sediment.     

Microstructure of nickel nanoparticles embedded in carbon films: case study on annealing effect by micromorphology analysis

The presented study is aimed at analyzing the surface texture of amorphous hydrogenated carbon layers containing nickel nanoparticles (Ni‐NPs@a‐C:H) within their structure, which were deposited by Radio Frequency (RF) sputtering and RF‐Plasma Enhanced Chemical Vapor Deposition (RF‐PECVD) methods on glass substrates. Prepared films were then used as research material following their annealing at two different temperatures of 250 °C and 350 °C in an inert argon atmosphere. Series of height samples were taken with the help of atomic force microscopy (AFM) operating in a non‐contact mode and examined in order to determine their fractal characteristics. Raw AFM data were first plane‐fitted to remove the surface bow exhibiting the so‐called residual surface, and then numerically processed to calculate the Areal Autocorrelation Function (AACF), which was later used to compute the Structure Function (SF). The log–log plots of the latter served for calculation of fractal properties of surfaces under investigation, including fractal dimension D, and pseudo‐topothesy K. The analysis of 3‐D surface texture helps to understand their essential characteristics and their implications as well as graphical models and their implementation in computer simulation. Copyright © 2016 John Wiley & Sons, Ltd.     

Synthesis of pyranopyrazoles,benzopyrans, amino-2-chromenes and dihydropyrano[<Emphasis Type="Italic">c</Emphasis>]chromenes using ionic liquid with dual Brønsted acidic and Lewis basic sites

An efficient ionic liquid with both Brønsted acidic and Lewis basic sites, namely 1,4-dimethyl-1-(4-sulphobutyl)piperazinium hydrogen sulphate (IL1), was synthesised and characterised. IL1 is a “green”, homogeneous and reusable catalyst for: i) the synthesis of pyranopyrazoles (Va-Vj)and benzopyrans (VIa-VIj and VIIa-VIIf) at ambient temperature under solvent-free conditions and ii) the synthesis of amino-2-chromenes (VIIIa-VIIIi and IXa-IXi) and dihyropyrano[c]chromenes (Xa-Xi) at 80 °C under solvent-free conditions. The reactions were rapid with excellent product yields. In addition, the double Brønsted acid, 1,4-dimethyl-1,4-bis(4-sulphobutyl)piperazinium hydrogen sulphate (IL2), was prepared to evaluate the cooperation efficiency of their Brønsted acidic and Lewis basic sites as compared with the double Brønsted acidic sites in IL1.     

Efficient removal of hexavalent chromium and lead from aqueous solutions by s‐triazine containing nanoporous polyamide

s‐Triazine containing dicarboxylic acid was synthesized. Then, it was reacted with 1,3‐phenylenediamine in molten tetrabutylammonium bromide to formed soluble aromatic polyamide with good yield and moderate inherent viscosity of 0.35 dL g^?1. The solubility and flexibility of polyamides are low. So, we used ether group such as di(4‐aminephenyl) ether in building polyamide. The structure of monomer and polymer was confirmed by Fourier transform infrared spectroscopy, elemental analysis, and proton nuclear magnetic resonance techniques. Thermogravimetric analysis was used to evaluate the thermal properties of synthesized polyamide, and their results show that this polymer had a good thermal stability. The surface morphology of s‐triazine containing polyamide was studied by field emission‐scanning electron microscopy and transmission electron microscopy, and the results show that it has a porous morphology and moderate Brunauer–Emmett–Teller specific surface (367 m² g^?1). It was further investigated for Pb (II) and Cr(VI) ion removal by optimizing the parameters including pH and contact time. The maximum uptakes of Pb(II) and Cr(VI) at pH 5.0 and pH 4.0 are 57% and 76%, respectively. Also, sorption kinetics of this polymer was investigated. Copyright © 2017 John Wiley & Sons, Ltd.     

Temporary shape development in shape memory nanocomposites using magnetic force

Direct mechanical force is used to create a temporary shape in shape memory polymers. This can become difficult in situations where the sample is not directly accessible such as interior in the body. In these cases it is not possible to use a direct mechanical force to deform the sample into temporary shape; therefore other alternative routes should be proposed. The magnetic force is a good candidate for inducing remote deformation. The ability of magnetic field to cause deformation in soft matters has already been revealed. To prove the hypothesis of using magnetic force to create temporary shape, magnetic field active shape memory polymeric nanocomposites were manufactured by incorporation of NdFeB ferromagnetic micro particles in a nanocomposite based on crosslinked low density polyethylene loaded with 2 wt.% of organoclay. The results indicate that as the NdFeB content increases, the reversible temporary deformation induced in the samples by the magnetic force increases. The effect of NdFeB concentration on the shape recovery progress and the possibility of heat induction in NdFeB filled samples through the application of an alternating magnetic field were also examined.     

Tin(II) Halide Insertion or Halogen Exchange in the Reactions of Dihaloplatinum(II) Complexes with Tin(II) Halide

Reactions of SnCl₂ with the complexes cis‐[PtCl₂(P₂)] (P₂=dppf (1,1′‐bis(diphenylphosphino)ferrocene), dppp (1,3‐bis(diphenylphosphino)propane=1,1′‐(propane‐1,3‐diyl)bis[1,1‐diphenylphosphine]), dppb (1,4‐bis(diphenylphosphino)butane=1,1′‐(butane‐1,4‐diyl)bis[1,1‐diphenylphosphine]), and dpppe (1,5‐bis(diphenylphosphino)pentane=1,1′‐(pentane‐1,5‐diyl)bis[1,1‐diphenylphosphine])) resulted in the insertion of SnCl₂ into the Pt? Cl bond to afford the cis‐[PtCl(SnCl₃)(P₂)] complexes. However, the reaction of the complexes cis‐[PtCl₂(P₂)] (P₂=dppf, dppm (bis(diphenylphosphino)methane=1,1′‐methylenebis[1,1‐diphenylphosphine]), dppe (1,2‐bis(diphenylphosphino)ethane=1,1′‐(ethane‐1,2‐diyl)bis[1,1‐diphenylphosphine]), dppp, dppb, and dpppe; P=Ph₃P and (MeO)₃P) with SnX₂ (X=Br or I) resulted in the halogen exchange to yield the complexes [PtX₂(P₂)]. In contrast, treatment of cis‐[PtBr₂(dppm)] with SnBr₂ resulted in the insertion of SnBr₂ into the Pt? Br bond to form cis‐[Pt(SnBr₃)₂(dppm)], and this product was in equilibrium with the starting complex cis‐[PtBr₂(dppm)]. Moreover, the reaction of cis‐[PtCl₂(dppb)] with a mixture SnCl₂/SnI₂ in a 2 : 1 mol ratio resulted in the formation of cis‐[PtI₂(dppb)] as a consequence of the selective halogen‐exchange reaction. ³¹P‐NMR Data for all complexes are reported, and a correlation between the chemical shifts and the coupling constants was established for mono‐ and bis(trichlorostannyl)platinum complexes. The effect of the alkane chain length of the ligand and Sn^II halide is described.