Synthesis,Crystal Structure,Thermal and Explosive Properties of [Cd(SCZ)3(H2O)](PA)2·3H2O (SCZ = Semicarbazide,PA = Picrate)

The heptacoordinate transition metal coordination compound [Cd(SCZ)₃(H₂O)](PA)₂ · 3H₂O ( 1 ) with the ligand semicarbazide (SCZ) and the counteranion picrate (PA) was synthesized and characterized by elemental analysis and FTIR spectroscopy. Single‐crystal X‐ray diffraction analysis revealed that 1 crystallizes in the monoclinic space group P21/c. The Cd²⁺ ion is heptacoordinated by three SCZ groups and a water molecule. SCZ presents typical bidentate coordination modes. The thermal decomposition mechanism of 1 was studied by differential scanning calorimetry (DSC), which revealed that complex 1 exhibits three small endothermic and two large exothermic processes. The non‐isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa‐Doyle's method, respectively. The heat of combustion was measured by oxygen bomb calorimetry. The enthalpy of formation, the critical temperature of thermal explosion, the entropy of activation (ΔS^≠), the enthalpy of activation (ΔH^≠), and the free energy of activation (ΔG^≠) were also calculated. Sensitivity tests revealed that 1 is insensitive to mechanical stimuli.     

电子束辐照下呋喃西林代谢产物降解的质谱检测

提出用电子束辐照技术降解去除水溶液中的呋喃西林代谢形成的氨基脲（SC）.采用LC-MS/MS方法分析SC含量变化.结果表明：当SC质量浓度小于0.67mg/L、辐照强度大于8 kGy时,SC降解率高达90%以上,没有检测到明显的降解产物.可见,电子束辐照降解法是-种简便、有效的有机污染物去除方法.     

A facile and convenient approach to the synthesis of 3,5-diaryl-1<Emphasis Type="Italic">H</Emphasis>-pyrazoles

A simple and convenient one-pot synthesis route is described for the synthesis of 3,5-diaryl-1H-pyrazoles in short reaction times from the reaction of α-epoxyketones with semicarbazide hydrochloride under mild conditions. Correspondence: Farzad Nikpour, Department of Chemistry, Faculty of Sciences, University of Kurdistan, P.O. Box 66315-416, Sanandaj, Iran.     

Green and Efficient Synthesis of 3-Pyrazolyl Indoles in Water

A green and efficient synthesis of 3-pyrazolyl indoles was developed by the cyclocondensation reaction of β-ethylthio-β-indolyl-α,β-unsaturated ketones with semicarbazide hydrochloride as hydrazine equivalent in the presence of 3 equiv. of PEG-400(1a/PEG mole ratio of 1:3) in reflux water. This procedure did not require toxic hydrazine and product purification, eliminating the use of toxic liquid chemicals.     

Synthesis of the first nanomagnetic particles with semicarbazide‐based acidic ionic liquid tag: an efficient catalyst for the synthesis of 3,3′‐(arylmethylene)bis(4‐hydroxycoumarin) and 1‐carbamato‐alkyl‐2‐naphthol derivatives under mild and green conditions

Semicarbazide functionalized with chlorosulfonic acid on the surface of silica‐coated magnetic nanoparticles, {Fe₃O₄@SiO₂@(CH₂)₃Semicarbazide‐SO₃H/HCl}, as a novel magnetic Brønsted acid catalyst according to the aims of green chemistry was synthesized and fully characterized using Fourier transform infrared, UV–visible and energy‐dispersive X‐ray spectroscopies, X‐ray diffraction, scanning electron, transmission electron and atomic force microscopies and thermogravimetric analysis. The capability and excellent activity of this nanoparticle catalyst were exhibited in the synthesis of two series of compounds with important biological activities, namely 3,3′‐(arylmethylene)bis(4‐hydroxycoumarin) and 1‐carbamato‐alkyl‐2‐naphthol derivatives, under mild, green and solvent‐free conditions. To the best of our knowledge, this is the first study of the synthesis and application of {Fe₃O₄@SiO₂@(CH₂)₃Semicarbazide‐SO₃H/HCl} as Brønsted acid solid magnetic nanoparticles. Consequently the present study can open up a novel and promising intuition in the sequence of logical design, synthesis and applications of task‐specific Brønsted acid magnetic nanoparticle catalyst with favourable properties as a full‐fledged efficient material for sustainable approaches. Copyright © 2016 John Wiley & Sons, Ltd.     

Syntheses,Crystal Structures,and Thermal Properties of Energetic Semicarbazide Salt,Manganese(II) Salt,and Coordination Compound of 3,5‐Dinitrobenzoic Acid

Nitro compounds have been actively researched as driven by their potential to be high‐performing energetic materials. Herein, three new nitro compounds including semicarbazide 3,5‐dinitrobenzoate, (SCZ)(DNBA), manganese 3,5‐dinitrobenzoate dihydrate, [Mn(DNBA)₂(H₂O)₂]_n, and bis(semicarbazide) manganese(II) 3,5‐dinitrobenzoate, Mn(SCZ)₂(DNBA)₂, were synthesized and characterized by elemental analysis, IR spectroscopy, and single‐crystal X‐ray diffraction analysis. The results indicated that the above mentioned compounds are ionic, polymeric, and molecular in nature, respectively. Moreover, their thermal decomposition properties were assessed by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Their non‐isothermal reaction kinetics parameters, critical temperature of thermal explosion (T_bp), entropy of activation (ΔS^≠), enthalpy of activation (ΔH^≠), and free energy of activation (ΔG^≠) of the exothermic decomposition process were also calculated. Results suggest that there was a relationship between the structure and thermal stability.     

纳米二氧化硅负载FeCl3作为一种高效多相催化剂用于合成1,2,4-三嗪衍生物（英文）

The one‐pot synthesis of a series of 1,2,4‐triazines from the reactions of semicarbazide or thiosemi‐carbazide with various α,β‐dicarbonyl compounds under reflux conditions in a EtOH‐H2O (9:1) mixture as solvent and catalyzed by nano‐sized silica supported FeCl3 (FeCl3@SiO2) was investigat‐ed. The FeCl3 content of the catalyst was measured by atomic absorption to get the adsorption ca‐pacity. The reactions gave high yields of the product and the catalyst was easily separated and re‐used for successive reaction runs without significant loss of activity.     

Syntheses of 4‐(5‐oxo‐1,2,4‐triazol‐3‐yl)‐sydnones and 4‐(4‐arylamino‐5‐oxo‐1,2,4‐triazol‐3‐yl)‐sydnones from Sydnone Derivatives and Their Fragments

4‐(5‐oxo‐1,2,4‐triazol‐3‐yl)‐sydnones 11 and 4‐(4‐arylamino‐5‐oxo‐1,2,4‐triazol‐3‐yl)‐sydnones 13 have been obtained from a‐chloroformylarylhydrazine hydrochloride 2 . Moreover, the intermediates, including 3, 4 , 9 and 10 , in this study are synthetically informative and valuable. It is also noteworthy that three reactants, 1, 2 and sydnonecarbaldehydes, were prepared from sydnone derivatives and their fragments. The oxidative cyclizations of sydnonecarbaldehyde semicarbazones 9 and carbazones 10 with two different oxidizing agents (Cu(ClO₄)₂ and Fe(ClO₄)₃) have been extensively examined. The reaction time and the yields of cyclizations were affected by the substituents of semicarbazones 9 and carbazones 10.     

Simulation of polyurethane/activated carbon surface interactions

The influence of interfacial structure on interfacial properties between activated carbon filler and surrounding organic matrix of composites has been studied by infrared and NMR spectroscopy. Urea, semicarbazide and ethylurethane, component parts of polyurethane, have been used as organic model compounds in order to predict the interactions between the activated carbon surface and polar groups of real polyurethane molecule. It was shown that organic matrix/activated carbon interphase presented a region where the filler and matrix phases were chemically and/or physically combined. The spectra of the organic matrix undergo significant changes with increase of carbon content. Due to the surface reactive functionalities the activated carbon is considered not only as filler, influenced on the sorption properties of the composition, but also as a physicochemical modifier of the polyurethane matrix.     

Synthesis and Antibacterial Evaluation of Some Semicarbazides and 1,2,4‐Triazol‐5‐Ones Containing Thiophene Moieties

In this study, some 3‐(thiophen‐2‐ylmethyl)‐4‐substituted‐4,5‐dihydro‐1H‐1,2,4‐triazol‐5‐one derivatives were synthesized by the cyclization reaction of 1‐(thiophen‐2‐ylacetyl)‐4‐substituted semicarbazide derivatives in alkaline medium or in the immediate reaction of thiophen‐2‐yl‐acetic acid hydrazide with isocyanates. The structures of all new compounds were confirmed by analytical and spectroscopic methods. Selected derivatives were evaluated in vitro against several species of aerobic bacteria. Some of them showed activity against S. pyogenes, P. aeruginosa and S. aureus.