新的金属氧化物纳米催化剂CuO-ZnO高效催化醇化学选择性乙酰化（英文）

A new method has been developed for the chemoselective acetylation of alcohols with acetic anhy‐dride in the presence of phenols using a novel,recyclable Cu O‐Zn O nanocatalyst.The catalyst was synthesized using the co‐precipitation method and characterized by N2 adsorption‐desorption,X‐ray diffraction,scanning electron microscopy,transmission electron microscopy and energy dis‐persion scanning analyses.Furthermore,this catalyst could be recycled up to six times without significant loss in its activity.     

Heterocycles [h]-fused to 4-oxoquinoline-3-carboxylic acid. Part VII: synthesis of some 6-oxoimidazo[4,5-h]quinoline-7-carboxylic acids and esters

Abstract  

A series of ethyl 2-(substituted)-9-cyclopropyl-4-fluoro-6-oxo-1H-imidazo[4,5-h]quinoline-7-carboxylates has been prepared from ethyl 7,8-diamino-1,4-dihydroquinoline-3-carboxylate via thermally induced reactions with model alkanoic acids or via microwave-assisted cyclocondensation with some arene carboxaldehydes. Acid-catalysed hydrolysis of the resulting ester derivatives furnished the corresponding imidazoquinoline-7-carboxylic acids. The structures of these new acid and ester derivatives are based on microanalytical and spectral (IR, MS, and NMR) data.     

Synthesis and fabrication of (1 − x)ZnAl2O4–xSiO2 thin films to be applied as patch antennas

Zinc aluminate compounds have been dispersed in silica matrix prepared by sol-gel method with different compositions for (1 ? x)ZnAl₂O₄–xSiO₂. Continuous stirring of ethylene glycol solution contained zinc nitrate, aluminium nitrate and silicon dioxide to produces gel precursor. Structural and morphological studies of (1 ? x)ZnAl₂O₄–xSiO₂ thin films were examined by field emission scanning electron microscopy (FESEM) and X-ray diffractometer (XRD) analysis. The FESEM images showed the spherical structures with porosity for (1 ? x)ZnAl₂O₄–xSiO₂ thin films. XRD analysis indicated that the crystallite size for (1 ? x)ZnAl₂O₄–xSiO₂ increased from 39.79 to 44.34 nm. Fourier transform infra-red analysis showed that the existence of H₂O molecules and the presence of nitrate group within the samples. Dielectric permittivity (ε _r ) of (1 ? x)ZnAl₂O₄–xSiO₂ samples were measured within frequency range from 1 Hz to 1 MHz. The dielectric permittivity, ε _r decreased as frequency was applied to the sample. The performance of the patch antenna can be measured using return loss analysis. The highest result shows that the patch antenna resonated at frequency 3.46 GHz and gives ?14.25 dB return loss bandwidth.     

Detection of explosives and their degradation products in soil environments

Polynitro organic explosives [hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) and 2,4,6-trinitrotoluene (TNT)] are typical labile environmental pollutants that can biotransform with soil indigenous microorganisms, photodegrade by sunlight and migrate through subsurface soil to cause groundwater contamination. To be able to determine the type and concentration of explosives and their (bio)transformation products in different soil environments, a comprehensive analytical methodology of sample preparation, separation and detection is thus required. The present paper describes the use of supercritical carbon dioxide (SC-CO2), acetonitrile (MeCN) (US Environmental Protection Agency Method 8330) and solid-phase microextraction (SPME) for the extraction of explosives and their degradation products from various water, soil and plant tissue samples for subsequent analysis by either HPLC-UV, capillary electrophoresis (CE-UV) or GC-MS. Contaminated surface and subsurface soil and groundwater were collected from either a TNT manufacturing facility or an anti-tank firing range. Plant tissue samples were taken fromplants grown in anti-tank firing range soil in a greenhouse experiment. All tested soil and groundwater samples from the former TNT manufacturing plant were found to contain TNT and some of its amino reduced and partially denitrated products. Their concentrations as determined by SPME-GC-MS and LC-UV depended on the location of sampling at the site. In the case of plant tissues, SC-CO2 extraction followed by CE-UV analysis showed only the presence of HMX. The concentrations of HMX (<200 mg/kg) as determined by supercritical fluid extraction (SC-CO2)-CE-UV were comparable to those obtained by MeCN extraction, although the latter technique was found to be more efficient at higher concentrations (>300 mg/kg). Modifiers such as MeCN and water enhanced the SC-CO2 extractability of HMX from plant tissues.     

Three-dimensional pillar-layered copper(II) metal-organic framework with immobilized functional OH groups on pore surfaces for highly selective CO2/CH4 and C2H2/CH4 gas sorption at room temperature

A new three-dimensional microporous metal-organic framework Cu(BDC-OH)(4,4'-bipy)·G(x) (UTSA-15; H(2)BDC-OH = 2-hydroxy-benzenedicarboxylic acid, 4,4'-bipy =4,4'-bipyridine, G = guest molecules) with functional -OH groups on the pore surfaces was solvothermally synthesized and structurally characterized. UTSA-15 features a three-dimensional structure having 2D intercrossed channels of about 4.1 × 7.8 and 3.7 × 5.1 ?(2), respectively. The small pores and the functional -OH groups on the pore surfaces within the activated UTSA-15a have enabled their strong interactions with CO(2) and C(2)H(2) which have been revealed in their large adsorption enthalpies of 39.5 and 40.6 kJ/mol, respectively, highlighting UTSA-15a as the highly selective microporous metal-organic framework for the CO(2)/CH(4) and C(2)H(2)/CH(4) gas separation with separation selectivity of 24.2 and 55.6, respectively, at 296 K.     

Analysis and development of structure-fragmentation relationships in withanolides using an electrospray ionization quadropole time-of-flight tandem mass spectrometry hybrid instrument

Structural elucidation and gas‐phase fragmentation of ten withanolides (steroidal lactones) were studied using a positive ion electrospray ionization quadropole time‐of‐flight mass spectrometry (ESI‐QqTOF‐MS/MS) hybrid instrument. Withanolides form an important class of plant secondary metabolites, known to possess a variety of biological activities. Withanolides which possess hydroxyl groups at C‐4, C‐5, C‐17, C‐20, and C‐27, and an epoxy group at C‐5/C‐6, were evaluated to determine the characteristic fragments and their possible pathways. ESI‐QqTOF‐MS (positive ion mode) showed the presence of the protonated molecules [M + H]⁺. Low‐energy collision‐induced dissociation tandem mass spectrometric (CID‐MS/MS) analysis of the protonated molecule [M + H]⁺ indicated multiple losses of water and the removal of the C‐17‐substituted lactone moiety affording the [M + H–Lac]⁺ product ion as the predominant pathways. However, withanolides containing a hydroxyl group at C‐24 of the lactone moiety showed a different fragmentation pathway, which include the loss of steroidal part as a neutral molecule, with highly diagnostic ions at m/z 95 and 67 being generated from the cleavage of lactone moiety. Our results also determined the influence of the presence and positions of hydroxyl and epoxy groups on product ion formation and stability. Moreover, the knowledge of the fragmentation pattern was utilized in rapid identification of withanolides by the LC/MS/MS analysis of a Withania somnifera extract. Copyright © 2010 John Wiley & Sons, Ltd.     

Novel,One-Pot,Three-Component,Regioselective Synthesis of Fluorine-Containing Thiazole and Bis-3H-thiazole Derivatives Using Polyvinyl Pyridine as Heterogeneous Catalyst,and Evaluation of Their Antibacterial Activity

A convenient, one-pot, three-component regioselective synthesis of novel 2,2′-(1,4-phenylene)-bis-(3-aryl-2-substituted imino-4-aryl-3H-thiazole) derivatives from 1,4-phenylene diisothiocyanate, aryl amines, and various phenacyl bromide, and also the regioselective synthesis of 3-alkyl-2-(aryl imino)-4-cyclopropyl-5-(2′-fluorophenyl)-thiazole derivatives from alkylisothiocyanate, aryl amines, and 2-bromo-2-(2-fluorophenyl)-1-cyclopropylethanone in the presence of poly-4-vinyl pyridine as heterogenous basic catalyst are described. This efficient method produced the products at room temperature with excellent yields (82–96%). The structures of all products were characterized by spectral and elemental analyses. The antimicrobial activity of the synthesized compounds was evaluated against Salmonella enterica, Micrococcus luteus, Bacillus subtilis, and Pseudomonas aeruginosa.     

Synthesis,characterization, thermal and luminescent properties of thiophenol-functionalized platinum(II) bis(acetylide) complexes

Transition Metal Chemistry - Two thiophenol-functionalized trans-platinum(II) bis(acetylide) complexes, having one thiophenol moiety in each alkenyl backbone with general formula...     

Click synthesis of 1,4-disubstituted-1,2,3-triazoles catalyzed by melamine-supported CuO nanoparticles as an efficient recyclable catalyst in water

Melamine-supported CuO nanoparticles (M-CuO nanocatalyst) are prepared as a new and efficient recyclable nanocatalyst for the regioselective synthesis of 1,2,3-triazoles in water. This new nanocatalyst was prepared by co-precipitation method and characterized by FT-IR spectral study, TGA, DSC, XRF, ICP-OES, XRD, SEM, EDS and BET analysis. A wide range of 1,4-disubstituted-1,2,3-triazoles were synthesized from reaction of benzyl halides or alkyl halides with phenyl acetylene and sodium azide in high yields. M-CuO nanocatalyst could be reused more than 6 times without considerable loss of its initial activity.