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961.
The novel complex [K(18-C-6)]2[Cd(mnt)2][18-C-6-18-crown-6,nmt=1,2-dicyanoethene-1,2-dithiolate,C2S2-(CN)2^2-] was synthesized and characterized by elemental analysis,IR spectrum and X-ray diffraction analysis.The complex displays two-dimensional network structure of [K(18-C-6)] complex segments and [Cd(nmt)2] complex segment bridged by S-K-S,S-K-N and N-K-N interactions between adjacent[K(18-C-6)] and [Cd(mnt)2]units. 相似文献
962.
一种新的环糊精衍生物手性固定相的合成及其在对映异构体过量值测定中的应用 总被引:4,自引:0,他引:4
以 β 环糊精为原料 ,合成了一种新的环糊精衍生物 2 ,6 二 O 苄基 3 O 戊酰基 β 环糊精 ,用核磁氢谱和红外光谱对产物进行了表征 ,并将所得环糊精衍生物用作毛细管气相手性固定相制备成柱 ,用于 2 ,4 二氯苯乙酮的不对称催化氢化产物 2 ,4 二氯苯乙醇和反式 2 己烯醇的Sharpless环氧化产物 反式 3 正丙基环氧乙烷甲醇的对映异构体过量值 (e.e .值 )测定和催化反应评价 ,取得了很好的结果。 相似文献
963.
Fabrication of hollow palladium spheres and their successful application to the recyclable heterogeneous catalyst for suzuki coupling reactions 总被引:25,自引:0,他引:25
Novel palladium hollow spheres were synthesized using silica spheres as a template, and they were successfully applied as recyclable heterogeneous catalysts for Suzuki cross coupling reactions. 相似文献
964.
Oleg V. Mikhailov Marina A. Kazymova Tatyana A. Shumilova Galina A. Chmutova Svetlana E. Solovieva 《Transition Metal Chemistry》2005,30(3):299-304
The complexing process proceeding in the NiII–thiocarbohydrazide (H2N–H–NC(=S)–NH–NH2)–propanone triple system in EtOH solution and nickel(II)hexacyanoferrate(II) gelatin-immobilized matrix has been studied. It has been found that in the first case, template synthesis leading, as a minimum, to formation of three coordination compounds of NiII with (N,N,S,S)-donor tetradentate ligands having NiL1, NiL2 and NiL3compositions where L1 is 4,6,6-trimethyl-2,3,7,8-tetraazanonen-3-di(thiohydrazide)-1,9, L2 is 4,6,6,12-tetrametyl-1,9-dithio-2,3,7,8,10,11-hexaazatridekadien-3,11-hydrazide-1 and L3 is 2,8,10,10,16-pentamethyl-5,13-dithio-3,4,6,7,11,12,14,15-octaazaheptadekatrien-2,7,15 is observed, whereas in the gelatin-immobilized matrix, a complexing process in the system considered does not occur. 相似文献
965.
G. J. Dear D. N. Mallett D. M. Higton A. D. Roberts S. A. Bird H. Young R. S. Plumb I. M. Ismail 《Chromatographia》2002,55(3-4):177-184
Summary In this paper we investigate the potential of alkyl-bonded silica monolithic columns for the isolation and identification
of drug-related components in biological fluids. Up to 6 columns have been connected in series to produce a chromatographic
system with up to 40,000 plates. This high-resolution chromatography system has been coupled to both MS and NMR to enable
efficient detection and characterisation of drug-related components in biological fluids. The use of six coupled columns has
been shown to give enhanced resolution over a high quality silica particulate column packed with 3 μm material which exhibits
the same back pressure. The effect of volume and mass load on the performance of monolithic columns for semi-preparative chromatography
of biological fluids has also been investigated. In these studies it was possible to inject up to 100 mL of neat urine with
no loss of chromatographic performance. Furthermore, upon re-testing, the columns showed similar chromatographic performance.
Again several columns were serially connected, producing enhanced resolution in the semi-preparative mode. 相似文献
966.
Heo YS Ryu JM Park SM Park JH Lee HC Hwang KY Kim J 《Experimental & molecular medicine》2002,34(3):211-223
Protein-tyrosine phosphatases (PTPs) constitute a family of receptor-like, and cytoplasmic enzymes, which catalyze the dephosphorylation of phosphotyrosine residues in a variety of receptors and signaling molecules. Together with protein tyrosine kinases (PTKs), PTPs are critically involved in regulating many cellular signaling processes. In this study, diverse compounds were screened for PTP inhibition and selectively screened for inhibitors with the end product inhibition properties. Among phosphate analogues and their derivatives for PTP inhibition, Keggin compounds phosphomolybdate (PM) and phosphotungstate (PT) strongly inhibited both PTP-1B and SHP-1, with K(i) values of 0.06-1.2 micromM in the presence of EDTA. Unlike the vanadium compounds, inhibition potencies of PM and PT were not significantly affected by EDTA. PM and PT were potent, competitive inhibitors for PTPs, but relatively poor inhibitors of Ser/Thr phosphatase. Interestingly, PM and PT did not inhibit alkaline phosphatase at all. The crystal structure of PTP-1B in complex with PM, at 2.0 A resolution, reveals that MoO(3), derived from PM by hydrolysis, binds at the active site. The molybdenium atom of the inhibitor is coordinated with six ligands: three oxo-ligands, two apical water molecules and a S atom of the catalytic cysteine residue. In support of the crystallographic finding, we observed that molybdenium oxides (MoO(3), MoO(2), and MoO(2)Cl(2)) inhibited PTP-1B with IC(50) in the range 5-15 micromM. 相似文献
967.
Yuan Ruo Cao ShuRui Chai YaQin Gao FengXian Zhao Qing Tang MingYu Tong ZhongQiang Xie Yi 《中国科学B辑(英文版)》2007,50(5):620-628
Alternate adsorption of positively charged colloid-Au nanoparticles (nano-Au⊕) and negatively charged hemoglobin (Hb) on L-cysteine (L-cys) modified gold electrode resulted in the assembly of {Hb/nano-Au⊕}n layer-by-layer films/L-cys modified gold electrode. The nano-Au⊕ was characterized by transmission electron micrograph (TEM) and microelectrophoresis. The modified electrode interface morphology was characterized by electrochemical impedance spectroscopy (EIS), atomic force mi- croscopy (AFM), cyclic voltammograms (CV) and chronoamperometry. Direct electron transfer between hemoglobin and gold electrodes was studied, and the apparent Michaelis-Menten constant ( km app) of the modified electrode was evaluated to be 0.10 mmol·L?1. Moreover, the higher activity of proteins in the nano-Au⊕ films could be retained compared with the electropolymerization membrane, since the pro- teins in nano-Au⊕ films retained their near-native structure. Direct electron transfer between hemoglo- bin and electrode and electrochemically catalyzed reduction of hydrogen peroxide on a modified elec- trode was studied, and the linear range was from 2.1×10-8 to 1.2 ×10?3 mol·L-1 (r = 0.994) with a detection limit of 1.1×10-8 mol·L-1 H2O2. 相似文献
968.
Fluorescein has an extremely low luminescence intensity in acidic aqueous media. However, when it was bound to proteins, subsequent increase of luminescence intensity took place. Furthermore, when a hydrophobic tail, such as aliphatic hydrocarbons, was introduced to fluorescein, more dramatic increase of luminescence intensity was observed upon binding to proteins. In the present study, by utilizing this luminescence enhancement, three hydrophobic fluorescein dyes (5-dodecanoyl amino fluorescein, 5-hexadecanoyl amino fluorescein, and 5-octadecanoyl amino fluorescein) were examined as noncovalent fluorescent stains of protein bands in sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). Effective incorporation of the dyes to proteins in gels was accomplished either simply by adding dyes at the protein fixation step, or by treating gels with a staining solution after the fixation. The sensitivity of this staining method using the fluorescein derivatives was approximately 1 ng/band for most proteins. For some cases, protein bands containing as low as 0.1 ng were successfully visualized. In addition, the detection sensitivity showed much less protein-to-protein variation than silver staining. This new staining method was also successfully applied to two-dimensional electrophoresis of rat brain proteins. Its overall sensitivity was comparable to that of silver staining. 相似文献
969.
Xiaobin Wang Xincan Fu Min Chen An Wang Jinghua Yan Yudong Mei Mengqi Wang Chunlong Yang 《中国化学快报》2019,30(7):1419-1422
A series of novel 1,3,5-thiadiazine-2-thione derivatives bearing a hydrazide moiety were designed, synthesized and evaluated for their biological activities against phytopathogenic fungi. The antifungal bioassays indicated that the title compound 5b impressively displayed the obvious selectivity and specificity aganist Rhizoctonia solani (Rs) in vitro and in vivo. The above researches provide a significant reference for the further structural optimization of 1,3,5-thiadiazine-2-thione derivatives bearing a hydrazide moiety as potential fungicides. 相似文献
970.
Chemistry related to three catalytic carbonylation reactions is discussed. Synthesis of diphenylurea from nitrobenzene, aniline,
and CO gives isolated yields above 98% at 100–120 °C and 15–60 bar of CO in the presence of a palladium (II) complex, PPh3 and NEt4Cl. Experimental evidence was provided to prove a new reaction stoichiometry and involvement of a carbamoyl intermediate.
In carbonylation of HCHO over ion exchange resin catalysts, reaction temperature, time, pressure, and solvent were important
variables to obtain high yields of methyl glycolate. Carbonylation of isobutylphenylethanol at 120°C and 40 bar of CO in the
presence of PdCl2−PPh3−HCl gives 98% yield of α-(4-isobutylphenyl) propionic acid (ibuprofen). Each catalyst component had a definite role that
is indispensable for an efficient overall reaction. 相似文献