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991.
Jacqueline Grewe Adelheid Hagenbach Brigitte Stromburg Roger Alberto Ezequiel Vazquez‐Lopez Ulrich Abram 《无机化学与普通化学杂志》2003,629(2):303-311
Novel rhenium(I) tricarbonyl complexes have been prepared by reactions of (Et4N)2[Re(CO)3Br3] with acetylpyridine benzoylhydrazone, Hapbhyd, di(2‐pyridyl)ketone benzoylhydrazone, Hpy2bhyd, bis(2‐pyridine)ketone, py2CO, and pyridinealdehyde terephtalaldehydebishydrazone, pytehyd. The ligands remain protonated when no supporting base is added and the following complexes have been isolated: [Re(CO)3Br(Hapbhyd)], [Re(CO)3Br(Hpy2bhyd‐py, hyd)], [Re(CO)3Br(Hpy2bhyd‐py1, py2)], [Re(CO)3Br(py2CO‐N, N)] and [Re(CO)3Br(pytehyd)]. Addition of triethyl amine results in deprotonation of Hapbhyd and the formation of [Re(CO)3(OH2)(apbhyd)], whereas Hpy2bhyd is hydrolysed and a rhenium complex with the monoanionic bis(2‐pyridyl)hydroxymethanolato ligand, {py2C(OH)O}‐, is formed. The same compound, [Re(CO)3{py2C(OH)O}], is obtained when triethyl amine and water are added to a mixture of (Et4N)2[Re(CO)3Br3] and py2CO. The air‐stable products have been studied by spectroscopic methods and X‐ray crystallography. 相似文献
992.
Selective hydrogenation of α,β‐unsaturated carbonyls into saturated carbonyls is important to obtain remunerative products. However, it is still a challenge to achieve high activity and selectivity under mild conditions. Herein, Pd, Ir and bimetallic Pd‐Ir nanoparticles were uniformly deposited with high dispersity on the surface of SiC by a facile impregnation method, respectively. The as‐prepared Pd/SiC catalysts efficiently hydrogenate cinnamaldehyde to hydrocinnamaldehyde at room temperature and atmospheric pressure, and the activity of Pd/SiC is observed further enhanced by adding Ir component (conversion of 100%). In addition, the dependence of Pd‐Ir catalyst activity on Pd/Ir molar ratio confirms a synergistic effect between Ir and Pd, which originates from the electron transfer between Pd and Ir. 相似文献
993.
William J. Orts Geoffrey A. R. Nobes Gregory M. Glenn Gregory M. Gray Syed Imam Bor‐Sen Chiou 《先进技术聚合物》2007,18(8):629-635
Blends of thermoplastic starch with poly(ethylene‐co‐vinyl alcohol) copolymer (EVOH) were melt extruded with water/glycerol as plasticizer and a series of amino acid additives. The biggest factor in end‐use mechanical properties proved to be the relative humidity (RH) during storage. Plasticized starch‐EVOH blends stored at 0 and 50% RH changed significantly over time, with, for example, the tensile strength (TS) of the glycerol‐plasticized blend increasing from 4.7 to 26.3 MPa over 8 weeks when maintained at 0% RH. In contrast, the TS of this same sample stored at 75% RH remained unchanged for 8 weeks. Amino acids provided relatively minor, but significant changes in mechanical properties with time. Based on TS, elongation‐to‐break, and modulus, it may be concluded that β‐alanine, sarcosine, and L ‐proline were more effective than glycerol at maintaining strong flexible blends. Increases in crystallinity and changes in morphology with time, as described by modulated DSC were correlated to these changes in mechanical properties. Published in 2007 by John Wiley & Sons, Ltd. 相似文献
994.
Silvia E. Asías Ana M. Bruno Diego A. Dominici Mariela Bollini Carlos H. Gaozza 《Journal of heterocyclic chemistry》2003,40(1):107-112
In order to find new antimalarial drugs, an exploration about the chemical properties of the starting compounds 3‐amino‐6‐chloro‐4‐phenyl‐1H‐quinolin‐2‐one ( 1 ) and 3‐amino‐4‐methyl‐1H‐quinolin‐2‐one ( 2 ) was developed. Acylation with acyl chloride, sulfonyl chloride and acetic anhydride were carried out. Despite a previous report [2], when acetyl chloride or acetic anhydride were assayed on 1 , only the diacetyl derivative 7 was obtained. When this compound was heated at reflux temperature in a mixture of acetic acid and acetic anhydride, it was transformed in the oxazoloquinoline 8 . Further reactions of the acyl derivatives with diazomethane afforded 1‐methylated compounds. Compound 2 gave the imine 16 by condensation with 4‐nitrobenzaldehyde. 相似文献
995.
Kristian Lappalainen Katariina Yliheikkil Adnan S. Abu‐Surrah Mika Polamo Markku Leskel Timo Repo 《无机化学与普通化学杂志》2005,631(4):763-768
Iron(II) and cobalt(II) complexes ( 7 ‐ 15 ) based on new aldimine 2, 6‐bis[(imino)methyl]pyridine ( 1 , 2 , 4 , 6 ) and ketimine (2, 6‐bis[(imino)ethyl]pyridine ( 3 , 5 ) ligands with bulky chiral aliphatic or aromatic terminal groups have been prepared and characterized by 1H NMR, 13C NMR, IR‐, mass spectroscopy (EI), and elemental analysis. The complex [CoCl2(BBoMP)]·1/2 CHCl3 ( 13 ) (BBoMP: 2, 6‐bis{(R‐(+)‐(bornylimino)‐methyl}pyridine) crystallizes in monoclinic space group P21 with cell dimensions: a = 7.6603(11) Å, b = 28.3153(14) Å, c = 13.537(2) Å, V = 2908.1(6) Å3, Z = 4. The coordination sphere around Co is distorted trigonal bipyramidal. 相似文献
996.
Characterisation of pitch by HPLC 总被引:1,自引:0,他引:1
Summary A new high performance liquid chromatography method for the characterisation of toluene-soluble fractions of pitches has been
developed. Although a chromatographic system typical of size exclusion chromatography was used, results indicate that, for
these structurally complex samples, separation does not follow the usual discrimination by molecular size. A differentiation
between several classes of polyaromatic hydrocarbons is achieved instead. Data are reported on the analysis of individual
standard polyaromatic hydrocarbons, showing that four different elution ranges can be observed: three ofcata-condensed compounds (Cata1, Cata2 and Cata3) and one ofperi-condensed compounds (Peri). Results are reported proving the capacity of this high performance liquid chromatography method
to distinguish between pitches of different origin and nature. It is also effective for the study of the chemical reactions
occurring during heat treatment. 相似文献
997.
The molar heat capacity of the azeotropic mixture composed of ethanol and toluene was measured by a high precision adiabatic calorimeter from 80 to 320 K. The glass transition and phase transitions of the azeotropic mixture were determined based on the heat capacity measurements. A glass transition at 103.350 K was found. A solid-solid phase transition at 127.282 K, two solid-liquid phase transitions at 153.612 and 160.584 K were observed, which correspond to the transition of metastable crystal to stable crystal of ethanol and the melting of ethanol and toluene, respectively. The thermodynamic functions and the excess ones of the mixture relative to the standard temperature 298.15 K were derived based on the relationships of the thermodynamic functions and the function of the measured heat capacity with respect to temperature. 相似文献
998.
A very sensitive flow system for the direct determination of copper in natural waters based on spectrophotometric detection 总被引:1,自引:0,他引:1
A very sensitive flow injection method with spectrophotometric detection has been developed for the on-line determination of copper in natural waters. The method exhibits a limit of detection three times lower than the most sensitive direct spectrophotometric method previously described and then allows the direct and simple in situ determination of copper in most natural waters.The method was based on the measurement of the absorbance of the coloured complex formed by copper with the chromogenic reagent di-2-pyridyl ketone benzoylhydrazone (dPKBH) in an alkaline medium. This complex presents stoichiometry 1:2 (Cu:dPKBH), and exhibits maximum absorbance at 370 nm. The manifold used was very simple, and consisted of two channels. The first one contained the sample while the second one contained the colorimetric reagent (3.3×10−4 M dPKBH in 10% ethanol), in a 1.6×10−2 M phosphate buffer solution at pH 8. The performance of the system was optimised by using both univariate and modified simplex methodologies. When modified simplex was used, the best signal was obtained for a sample injection volume of 529 μl, a reaction coil length of 1.29 m, and a reagent flow rate of 4.8 ml min−1. Under optimum conditions, the response was linear up to 3 mg l−1 copper, the equation of the straight line being y=0.314x+5.2×10−4 (r2=0.998). The method allowed a sampling frequency of 40 samples per hour and exhibited a precision of 2.11% (as R.S.D., n=11). The limit of detection was 4.6 μg l−1 (calculated as 3sb/m, where sb is the standard deviation of the y-intercept and m represents the slope of the straight line), and was therefore more sensitive than all the direct continuous methods reported previously.The method was successfully applied to the analysis of real water samples, with an average relative error of 5.32%. 相似文献
999.
Triazene‐substituted arylboronic esters were prepared readily from the corresponding aryl magnesium derivatives and shown to function as a new class of donor–acceptor‐substituted coupling reagents. The selective functionalization of these aromatic derivatives led to a wide variety of terphenyl derivatives in which the original bifunctional unit (often further substituted with another functional group) formed the central aromatic ring. The functionalized terphenyl derivatives were formed in two efficient cross‐coupling steps from the triazene‐substituted boronic esters: Suzuki cross‐coupling with an aryl halide was followed by BF3?OEt2‐induced palladium‐catalyzed coupling of the diazonium salt generated in situ from the triazene with an arylboronic acid. 相似文献
1000.
European Legislation establishes that the sum of the migration levels of bisphenol A diglycidyl ether (BADGE), its hydrolysis (BADGE.H2O and BADGE.2H2O) and chlorohydroxy (BADGE.HCl, BADGE.2HCl and BADGE.H2O.HCl) derivatives shall not exceed the limit of 1 mg/kg in foodstuffs or food simulants. A reversed-phase high-performance liquid chromatographic (RP-HPLC) method combined with mass spectrometry detection using atmospheric pressure chemical ionisation (APCI) is developed for the separation, quantification and identification of the interesting compounds. Quantification of the analytes was carried out in the single ion recording mode, once their characteristic masses were selected from their full spectra, by using an external calibration. The optimised method was suitable for the migration evaluation of these compounds in different samples. 相似文献