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91.
Magdy M. Gineinah Abd El-Kader M. Ismaiel Mohamed M. El-Kerdawy Richard A. Glennon 《Journal of heterocyclic chemistry》1990,27(3):723-726
Because of the close structural similarity between triazoloquinazolines and certain 5-membered ring mesoionic heterocycles, all of which possess antiinflammatory activity, we prepared several examples of the novel mesoionic 1,2,4-triazolo[4,3-c]quinazoline ring system for their therapeutic potential. These compounds can be prepared by the cyclization of the appropriately substituted 4-hydrazinoquinazolines with phosgene. When the mesoionic product was unsubstituted at the 5-position (i.e., quinazoline 2-position), it could only be isolated as its hydrochloride salt and not as its unstable free base. None of the mesoionic products were sufficiently stable in solution to allow for evaluation of their antiinflammatory activity. 相似文献
92.
Carballo R Casas JS García-Martínez E Pereiras-Gabián G Sánchez A Sordo J Vázquez-López EM 《Inorganic chemistry》2003,42(20):6395-6403
The reactions of methylacetoacetate and ethyl 2-methylacetoacetate thiosemicarbazones (H(2)L(A) and H(2)L(B), respectively) with [ReX(CO)(5)] and [ReX(CO)(3)(CH(3)CN)(2)] (X = Cl, Br) were explored under various experimental conditions. Besides the adducts fac-[ReX(CO)(3)(H(2)L)], in which the rhenium is coordinated to three carbonyl groups, the X anion, and the N,S-bidentate thiosemicarbazone ligand, the following complexes were also isolated: fac-[ReBr(CO)(3)(Hpyz(B))], the tetrameric complexes fac-[Re(pyz(A))(CO)(3)](4) and fac-[Re(pyz(B))(CO)(3)](4), and fac-[Re(pyz(B))(CO)(3)(H(2)O)] (where Hpyz(A) and Hpyz(B) are pyrazolones derived by cyclization of H(2)L(A) and H(2)L(B), respectively). The cyclization reactions were monitored by (1)H NMR spectroscopy and the complexes isolated were identified by elemental analysis, mass spectrometry, IR and (1)H NMR spectroscopy, and in some cases by X-ray diffractometry. The isolation and the full structural identification of the rather unusual fac-[ReBr(CO)(3)(Hpyz(B))], which contains the enol form of the pyrazolone ligand, affords new insight into the cyclization of thiosemicarbazones derived from beta-keto esters. 相似文献
93.
Owczarek E Kwiatkowski W Lemieszewski M Mazur A Rostkowski M Paneth P 《The Journal of organic chemistry》2003,68(21):8232-8235
Nitrogen, deuterium, halogen, and carbon kinetic isotope effects have been modeled for the Menshutkin reaction between methyl halides and substituted N,N-dimethylaniline at the HF/6-31G(d) level of theory augmented by the C-PCM continuum solvent model for several solvents. Systematic changes in geometries of the transition states and Gibbs free energies of activation have been found with phenyl ring substituents, solvent, and the leaving group. Kinetic isotope effects also change systematically; however, these changes are predicted to be small, inside the usual precision of the experimental measurements. On the contrary, no correlation has been found between the kinetic isotope effects and the Hammett constants for para substituents. Thus opposite to previous assumptions, our results indicate that kinetic isotope effects on the Menshutkin reaction cannot be used to predict the position of the transition state on the reaction coordinate. 相似文献
94.
Seyed Sajad Sajadikhah Malek Taher Maghsoodlou Nourallah Hazeri Sayyed Mostafa Habibi-Khorassani Anthony C.Willis 《中国化学快报》2012,23(5):569-572
An efficient green protocol is described for the preparation of highly functionalized piperidines via a one-pot five-component reaction between aromatic aldehydes,anilines andβ-ketoesters in the presence of oxalic acid dihydrate as catalyst in ethanol at ambient temperature.The structure as well as the relative stereochemistry of these compounds was confirmed by single X-ray crystallographic analysis. 相似文献
95.
Fereshteh Chekin Jahan‐Bakhsh Raoof Samira Bagheri Sharifah Bee Abd Hamid 《中国化学会会志》2012,59(11):1461-1467
We report a simple and effective strategy for fabrication of the nanocomposite containing chitosan (CS) and multiwall carbon nanotube (MWNT) coated on a glassy carbon electrode (GCE). The characterization of the modified electrode (CS‐MWNT/GC) was carried out using scanning electron microscopy (SEM) and UV–vis absorption spectroscopy. The electrochemical behavior of CS‐MWNT/GC electrode was investigated and compared with the electrochemical behavior of chitosan modified GC (CS/GC), multiwalled carbon nanotube modified GC (MWNT/GC) and unmodified GC using cyclic voltammetry (CV) and electron impedance spectroscopy (EIS). The chitosan films are electrochemically inactive; similar background charging currents are observed at bare GC. The chitosan films are permeable to anionic Fe(CN)63?/4? (FC) redox couple. Electrochemical parameters, including apparent diffusion coefficient for the Fe(CN)63?/4? redox probe at FC/CS‐MWNT/GC electrode is comparable to values reported for cast chitosan films. This modified electrode also showed electrocatalytic effect for the simultaneous determination of D‐penicillamine (D‐PA) and tryptophan (Trp). The detection limit of 0.9 μM and 4.0 μM for D‐PA and Trp, respectively, makes this nanocomposite very suitable for determination of them with good sensitivity. 相似文献
96.
97.
98.
Malek T. Maghsoodlou Nourallah Hazeri Sayed M. Habibi-Khorassani Reza Heydari Ghasem Marandi Mojtaba Lashkari Khatereh Bagherpour Zahra Gharechaei 《Monatshefte für Chemie / Chemical Monthly》2010,39(5):351-356
Abstract
Synthesis of five phosphonato esters has been accomplished via reaction between dimethyl acetylenedicarboxylate and triphenyl phosphite in the presence of biological compounds such as theophylline, 4-hydroxypyrimidine, 2H-3,1-benzoxazine-2,4(1H)-dione, 2-chloroaniline, or 3-nitroaniline at ambient temperature. The configuration of the compounds was determined on the basis of coupling constants emerging from the Karplus equation. 相似文献99.
Bramanti E D'Ulivo L Lomonte C Onor M Zamboni R Raspi G D'Ulivo A 《Analytica chimica acta》2006,579(1):38-46
A new procedure is proposed for the sampling and storage of hydrogen sulphide (H2S) and volatile thiols (methanethiol or methyl mercaptan, ethanethiol and propanethiol) for their determination by liquid chromatography. The sampling procedure is based on the trapping/pre-concentration of the analytes in alkaline aqueous solution containing an organic mercurial probe p-hydroxymercurybenzoate, HO-Hg-C6H4-COO− (PHMB), where they are derivatized to stable PHMB complexes based on mercury-sulfur covalent bonds. PHMB complexes are separated on a C18 reverse phase column, allowing their determination by liquid chromatography coupled with sequential non-selective UV-vis (DAD) and mercury specific (chemical vapor generation atomic fluorescence spectrometry, CVGAFS) on-line detectors. PHMB complexes, S(PHMB)2CH3S-PHMB, C2H5S-PHMB and C3H7S-PHMB, are stable alt least for 12 h at room temperature and for 3 months if stored frozen (−20 °C).The best analytical figures of merits in the optimized conditions were obtained by CVGAFS detection, with detection limits (LODc) of 9.7 μg L−1 for H2S, 13.7 μg L−1 for CH3SH, 17.7 μg L−1 for C2H5SH and 21.7 μg L−1 for C3H7SH in the trapping solution in form of RS-PHMB complexes, the relative standard deviation (R.S.D.) ranging between 1.0 and 1.5%, and a linear dynamic range (LDR) between 10 and 9700 μg L−1. Conventional UV absorbance detectors tuned at 254 nm can be employed as well with comparable R.S.D. and LDR, but with LODc one order of magnitude higher than AFS detector and lower specificity. The sampling procedure followed by LC-DAD-CVGAFS analysis has been validated, as example, for H2S determination by a certified gas permeation tube as a source of 3.071 ± 0.154 μg min−1 of H2S, giving a recovery of 99.8 ± 7% and it has been applied to the determination of sulfur compounds in real gas samples (biogas and the air of a plant for fractional distillation of crude oil). 相似文献
100.
Bartosz Tylkowski Malgorzata Pregowska Emilia Jamowska Ricard Garcia-Valls Marta Giamberini 《European Polymer Journal》2009,45(5):1420-1432
Microcapsules based on a new liquid crystalline lightly cross-linked polyamide, in which the state of order can be triggered by means of external stimuli, such as temperature and light, were prepared by interfacial polymerization. This polyamide exhibited a nematic phase up to 166 °C and it started to decompose at 340 °C; morphological variations of the film were observed by Scanning Electron Microscopy in correspondence to the clearing temperature; moreover, by continuous irradiation with UV light at room temperature, the polymer underwent E–Z photoisomerization. The prepared microcapsules contained either toluene, or concentrated solutions of naphthalene or β-carotene, as the core; in all cases, their outer surface appeared smooth and dense, while heterogeneities could be seen on the inner face. Capsule diameter lay in the range 30–120 μm, depending on the encapsulated material, with quite narrow size distributions. To the authors’ knowledge, this is the first example of microcapsules whose shell is completely constituted by a liquid crystalline lightly cross-linked polymer. Release experiments of β-carotene were performed in water and in tetrahydrofuran. β-Carotene release in water at 20 °C was strongly influenced by UV irradiation: in the absence of irradiation, it was practically negligible while, when microcapsules were submitted to continuous irradiation with UV light, β-carotene was quickly released and reached 100% release after 5 min. Preliminary experiments concerning the effect of temperature and of a swelling solvent, such as THF, on release, were also performed. 相似文献