Design,preparation and characterization of Cu/GA/Fe3O4@SiO2 nanoparticles as a catalyst for the synthesis of benzodiazepines and imidazoles

The synthesis and characterization of an efficient and reusable nanocatalyst, Cu/GA/Fe₃O₄@SiO₂, obtained by ultrasonic‐assisted grafting of guanidineacetic acid on modified Fe₃O₄@SiO₂ core–shell nanocomposite spheres and subsequent immobilization of Cu(II), are described. The catalyst was characterized by means of X‐ray diffraction, scanning and transmission electron microscopies, energy‐dispersive X‐ray spectroscopy, elemental analysis, thermogravimetric analysis, Fourier transform infrared spectroscopy, vibrating sample magnetometry and inductively coupled plasma optical emission spectrometry. The prepared nanocatalyst facilitated an efficient and straightforward friendly procedure for the synthesis of benzodiazepines and imidazoles in ethanol and under solvent‐free conditions, respectively. The nanocatalyst can be easily recovered using a magnet and reused several times without any significant loss of activity. Copyright © 2016 John Wiley & Sons, Ltd.     

Study on an optical system with coherent laser array source and phase optimization in turbulent atmosphere

Model of an optical system with coherent laser array source and the piston phase optimized by the stochastic parallel gradient descent algorithm is established. With this model, theory of beam propagation through the optical system in turbulent atmosphere is analyzed, and the analytical formulas of the beam average intensity along the propagation path are derived. Strehl ratio of the received beam induced by intensity disorderly distribution and power efficiency of the received beam are introduced to evaluate performance of the optical system. Under the H-V 5/7 atmospheric turbulent model, performance of an optical system with determinate parameters was calculated, and the influences of the propagation distance and the laser wavelength were numerically analyzed, respectively.     

Influence of aspect ratio and anisotropy distribution in ordered CoNi nanowire arrays

The size effects on magnetic properties of nanowires arrays were studied varying the nanowires diameter and maintaining the same periodicity among them, for two different nominal compositions of Co and Ni in the alloy form. The competition among magnetocrystalline and shape anisotropies changes drastically from smallest to biggest diameters altering the easy axis direction. In the case of 75% of Co in alloy, experimental values of the effective anisotropy constant (K_eff) vary from positive to negative depending on the diameter, which means a reversal of the easy axis direction. For 50% of Co the shape anisotropy dominates over the magnetocrystalline for all studied diameters.     

Silica iodide catalyzed,ultrasound-promoted,one-pot four-component synthesis of novel 1,4,5,6-tetrahydropyridine-3-carboxylate derivatives

Silica iodide catalyzed, competent synthesis of 15 novel substituted-1,4,5,6-tetrahydropyridine-3-carboxylate derivatives was achieved by a one-pot four-component cyclocondensation of Meldrum's acid, aryl aldehydes, aromatic amines and ethyl acetoacetate under ultrasonic irradiation. In comparison to the conventional methods, our protocol is convenient, eco-friendly and offers several benefits such as: mild conditions, high yields, shorter reaction time and ease in product isolation.     

Zinc‐containing ionic liquid as a dual solvent‐catalyst in base‐free condensations under ultrasonic irradiation

In this study, natural‐based ionic liquid (IL) using caffeine (Caff), trietahnolamine (TEA) and ZnBr₂, [Caff‐TEA]⁺[ZnBr₃]^?, which features high catalytic activity and environmentally‐friendly nature was synthesized with melting point of 76 °C by a facile method. The synthesized [Caff‐TEA]⁺[ZnBr₃]^? has high catalytic activity as both of catalyst and solvent in condensation reactions for the synthesis of benzylidenes, bis‐hydroxyenones and xanthenes. Synthesized IL was characterized by proton nuclear magnetic resonance (¹HNMR), Fourier transform infrared spectroscopy (FT‐IR), X‐ray diffraction (XRD) and Energy‐dispersive X‐ray spectroscopy (EDX) analysis. Also synthesized heterocycles were characterized by FT‐IR, proton nuclear magnetic resonance (¹HNMR) and carbon nuclear magnetic resonance (¹³CNMR).     

Development and validation of a RP-HPLC method for Roflumilast and its degradation products

Roflumilast is a phosphodiesterase type 4 inhibitor that is administered orally as a long-term, in the clinical treatment of chronic obstructive pulmonary disease and asthma. Launched in 2010 for the European market, it currently does not have an official monograph. Here, a reproducible gradient RP-HPLC method was developed and validated for the separation and determination of Roflumilast in the presence of its six major degradation products. Separation was performed on a C₁₈ analytical column (250?×?4.6?mm, 5?µm) with a mobile phase-A of ACN and a phase-B of ammonium acetate buffer (5?mM, pH 4.2) containing triethylamine (0.5% v/v). The most effective RP-HPLC gradient program was determined to be 0/80, 35/10, 36/80, 40/80 (time in minutes/% mobile phase-B). The flow rate was 1.0?ml/min and the column temperature was 25°C. The success of separation of the degradation products with different chemical characteristics was obtained by extending the time of the gradient, changing the proportion of the mobile phases and increasing the velocity of the flow. Two detectors were evaluated for the identification of degradation products and Roflumilast: a diode-arrary detector and a charged aerosol detector. The inability of the charged aerosol detector to dectect one of the six degradation products indicated that the method developed with RP-HPLC and the diode-array detector was more suitable for Roflumilast analysis. The method was validated according to specificity, linearity, LOD, LOQ, accuracy, precision and robustness.     

Ultrathin Mn Doped Ni-MOF Nanosheet Array for Highly Capacitive and Stable Asymmetric Supercapacitor

In this study, we demonstrate that an Mn-doped ultrathin Ni-MOF nanosheet array on nickel foam (Mn_0.1-Ni-MOF/NF) serves as a highly capacitive and stable supercapacitor positive electrode. The Mn_0.1-Ni-MOF/NF shows an areal capacity of 6.48 C cm⁻² (specific capacity C: 1178 C g⁻¹) at 2 mA cm⁻² in 6.0 m KOH, outperforming most reported MOF-based materials. More importantly, it possesses excellent cycle stability to maintain 80.6 % capacity after 5000 cycles. An asymmetric supercapacitor device utilizing Mn_0.1-Ni-MOF/NF as the positive electrode and activated carbon as the negative electrode attains a high energy density of 39.6 Wh kg⁻¹ at 143.8 Wkg⁻¹ power density with a capacitance retention of 83.6 % after 5000 cycles.     

Hydrolytic polycondensation of trimethoxymethylsilane under ultrasonic irradiation

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Variations of the elastic constants of InSb near the covalent-metallic transition

Abstract

The pulse-echo-overlap method was used to measure the longitudinal and transverse wave velocities in single-crystal (100) and (111) samples of InSb up to 3 GPa at room temperature. The peculiar variations of the elastic constants were observed near the covalent-metallic transition.     

Proposition of a compensated pixelwise calibration for photonic infrared cameras and comparison to classic calibration procedures: Case of thermoelastic stress analysis

In this paper, we propose a compensated pixelwise calibration that integrates the effects of the camera housing temperature. The results of this calibration are compared on black body images to classic two points Non Uniformity Correction based calibrations, compensated or not. It is shown that the proposed approach leads to a significant improvement in the thermal resolution with a reduction in the mean error as well as the standard deviation. The approach is finally challenged on a real case measurement focusing on thermoelasticity. The gain in terms of accuracy measurement is highlighted by comparing the proposed calibration to classic calibrations and the scope of interest of this new calibration is discussed.