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1.
Three new 8-hydroxyquinoline derivatives, i.e. 5-[(4-styryl-benzylidene)-amino]-quinolin-8-ol (1), 5-[(4-bromo-2-fluoro-benzylidene)-amino]-quinoline-8-ol (2) and 2-[2-(9-ethyl-9H-carbazol-2yl)-vinyl]-quinolin-8-ol (3), and their metallic complexes were synthesized and identified by ultraviolet-visible (UV-Vis), 1H nuclear magnetic resonance (1H NMR), Fourier transform infrared spectrometer (FTIR), mass spectrometry (MS) spectra and elemental analyses. Their fluorescence
properties were studied by photoluminescence, which indicated that the luminescence wavelength of 5-and 2-substitued-8-hydroxyquinoline
derivatives shifted to red in comparison with that of 8-hydroxyquinoline. Meanwhile, the fluorescence lifetime of 2-[2-(9-ethyl-9H-carbazol-2yl)-vinyl]-quinolin-8-ol
and its zinc complex showed long lifetime in benzene solution.
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Translated from Chinese Journal of Organic Chemistry, 2007, 27(3): 402–408 [译自: 有机化学] 相似文献
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Using cyclodextrin-capillary zone electrophoresis (CD-CZE), baseline separation of baclofen phaclofen, saclofen, and hydroxy-saclofen, potent gamma-aminobutyric acid(B) (GABA(B)) agonist or antagonists was achieved. A method for the enantioresolution of those analogs of GABA was developed using anionic cyclodextrins (highly sulfated CD or highly S-CD) as chiral selectors and capillaries dynamically coated with polyethylene oxide (PEO). With charged CDs we observed good resolutions due to the large electrophoretic mobility of these chiral selectors opposite to the mobility of the solutes. The highly S-alpha-CD and S-beta-CD were found to be complementary and the most effective complexing agent, allowing good enantiomeric resolution in short runtimes. The complete resolution was obtained using 25 mM phosphate buffer at pH 2.5 containing 3% w/v of highly S-alpha-CD or S-beta-CD at 25 degrees C with an applied field of 0.30 kV/cm. The apparent binding constants of the inclusion complexes were evaluated and the migration order was determined. A comparison was possible to investigate the importance of the anionic group of the molecules in the separations. The pK(a) values were determined for all four compounds in order to explain relative electrophoretic migration of the solutes. 相似文献
4.
Mónica Schwarz M. Carmen Rodríguez Dominico A. Guillén Carmelo G. Barroso 《Journal of separation science》2009,32(11):1782-1790
Brandy and other aged distillates are a rich source of polyphenols. For brandies, contact with wood during ageing makes an important contribution to their polyphenols content. This paper describes the use of a previously devised ultra performance LC (UPLC) method to study the polyphenols content of Brandy de Jerez. UPLC is a new technique in LC offering several potential advantages, especially the reduction of time. Analyses of brandy performed by HPLC were repeated by UPLC. A special UPLC analytical column (Acquity UPLC BEH C18 column, 100×2.1 mm), with a particle size of 1.7 μm, forms part of this system. Using the UPLC system enabled the time needed for analysis to be reduced to one tenth of the time needed in the conventional HPLC system. In conclusion, the separation factor results of the UPLC were compared to those obtained using HPLC methods; this demonstrated that simple, high efficiency UPLC gradients are viable and advantageous substitutes for traditional analysis of polyphenols in brandy by HPLC. The method enabled 14 phenolic compounds to be identified and determined in 33 different commercial brandies, and this allowed them to be differentiated in function of quality. 相似文献
5.
M. Mihit K. Laarej H. Abou El Makarim L. Bazzi R. Salghi B. Hammouti 《Arabian Journal of Chemistry》2010,3(1):55-60
The corrosion inhibition of copper and zinc in 0.1 M HNO3 by 1,2,3,4-tetrazole (TTZ) and some of its derivatives has been analysed in a comparative study. Two experimental techniques have been used such as weight-loss and electrochemical polarization measurements. The results obtained reveal that the addition of these compounds reduces preferentially the corrosion of Cu rather than that of Zn. The adsorption of tetrazolic compounds on a copper surface was more favourable than their adsorption on a zinc surface. Moreover the inhibition efficiency calculated for copper was found to attain 95% in the presence of 1-phenyl-5-mercapto-1,2,3,4-tetrazole (PMT) while it remains constant at 1% for all compounds tested using zinc as electrode. Relationship between molecular structure and their inhibition efficiency was elucidated by quantum chemical calculations using the density functional theory (DFT). 相似文献
6.
Fuping He Yiwang Chen Xiaohui He Muqing Chen Weihua Zhou Qing Wu 《Journal of polymer science. Part A, Polymer chemistry》2009,47(16):3990-4000
Vinyl‐type copolymerization of norbornene (NBE) and 5‐NBE‐2‐yl‐acetate (NBE‐OCOMe) in toluene were investigated using a novel homogeneous catalyst system based on bis(β‐ketonaphthylamino)Ni(II)/B(C6F5)3/AlEt3. The copolymerization behavior as well as the copolymerization conditions, such as the levels of B(C6F5)3 and AlEt3, temperature, and monomer feed ratios, which influence on the copolymerization were examined. Without combination of AlEt3, the catalytic bis(β‐ketonaphthylamino)Ni(II)/B(C6F5)3 exhibited very high catalyst activity for polymerization of NBE. Combination of AlEt3 in catalyst system resulted in low conversion for polymerization of NBE. For copolymerization of NBE and NBE‐OCOMe, involvement of AlEt3 in catalyst is necessary. Slight addition of NBE‐OCOMe in copolymerization of NBE and NBE‐OCOMe gives rise to significant increase of catalyst activity for catalytic system bis(β‐ketonaphthylamino)Ni(II)/B(C6F5)3/AlEt3. Nevertheless, excess increase of the NBE‐OCOMe content in the comonomer feed ratios results in decrease of conversion as well as activity of catalyst. The achieved copolymers were confirmed to be vinyl‐addition copolymers through the analysis of FTIR, 1H NMR, and 13C NMR spectra. 13C NMR studies further revealed the composition of the copolymer and the incorporation rate was 7.6–54.1 mol % ester units at a content of 30–90 mol % of the NBE‐OCOMe in the monomer feeds ratios. TGA analysis results showed that the copolymer exhibited good thermal stability (Td > 410 °C) and failed to observe the glass transitions temperature over 300 °C. The copolymers are confirmed to be noncrystalline by WAXD analysis results and show good solubility in common organic solvents. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 3990–4000, 2009 相似文献
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A green and efficient method for direct preparation of 3-cyanopyridine from aromatic aldehydes is reported. A series of novel 4-aryl-2-amino-6-(naphthalene-1-yl)-3-cyanopyridine derivates were successfully prepared by one-pot synthesis of three-component domino reactions including aromatic aldehydes, 1-acetylnaphthalene, and dicyanomethane in the presence of ammonium acetate in a solution of ethanol under microwave irradiation. This synthetic method for these compounds possesses many advantages including greater yield and shorter reaction times compared with traditional methods. The structures of these compounds were confirmed by means of high-resolution mass spectrometry, 1H NMR, 13C NMR, and infrared. Moreover, the results of their fluorescent spectra showed that these compounds have good fluorescence intensity excited by the visible light wavelength of 416 nm. 相似文献
8.
Nitrogen Derivates of Oxalic Acid as New Complexing Agents Heterocycles with a exocylic 1,4-diaza-1, 3-diene structure 5a–d have σ-bonding and π-backbonding properties similar to the diazadienes (DAD) 1 . The investigations of the molybdenum complexes 11 and 12 of the ligands 5 show a dominant σ-interaction and only a small π-backbonding, comparable with the compound (CO)4Mo(iPYC) 14 , a complex of pyridinecarbaldehyde isopropylimine (iPYC). The oxalamidine (TPOA) 4 (precursor of the heterocycles 5a–d ) are present in a s-trans (E/E)-form with two stable intra-molecular hydrogen bridges. 4 reacts with ferrous and cobaltous chloride to the polymer coordination compounds 8 and 9 . According to the diazadiene 1 oxalamadine 4 substitutes two carbonyls in Mo(CO)6 by formation of (CO)4Mo(TPOA) 10 . The coordinated ligand 4 shows in the complex 10 a s-cis(E/E)-form with respect to the free ligand and no H-bridges were observed. The crystal structures of TPOA 4 and (CO)4Mo(TPOA) 10 were determined. Cyclisation reactions on the coordinated oxalamidine are possible. 相似文献
9.
Brandão GP de Campos RC Luna AS de Castro EV de Jesus HC 《Analytical and bioanalytical chemistry》2006,385(8):1562-1569
A procedure for the determination of As in diesel, gasoline and naphtha at μg L−1 levels by GFAAS is proposed. Sample stabilization was achieved by the formation of three component solutions prepared by
mixing appropriate volumes of the samples propan-1-ol and nitric acid aqueous solution. This mixture resulted in a one-phase
medium, which was indefinitely stable. No changes in the analyte signals were observed over several days in spiked samples,
proving long-term stabilization ability. The use of conventional (Pd) and permanent (Ir) modification was investigated and
the former was preferred. Central composite design multivariate optimization defined the optimum microemulsion composition
as well as the temperature program. In this way, calibration using aqueous analytical solutions was possible, since the same
sensitivity was observed in the investigated microemulsion media and in 0.2% v/v HNO3. Coefficients of correlation larger than 0.999 and an As characteristic mass of 22 pg were observed. Recoveries (n=4) obtained from spiked samples were 98±4, 99±3 and 103±5%, and the limits of detection in the original samples were 1.8,
1.2 and 1.5 μg L−1 for diesel, gasoline and naphtha, respectively. Validation was performed by the analysis of a set of commercial samples by
independent comparative procedures. No significant difference (Student’s t-test, p<0.05) was observed between comparative and proposed procedure results. The total determination cycle lasted 4 min for diesel
and 3 min for gasoline and naphtha, equivalent to a sample throughput of 7 h−1 for diesel and 10 h−1 for gasoline and naphtha. 相似文献
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