新型2-氧代-1,2,4-三唑并[3,2-d][1,5]苯并氧氮杂类稠杂环的合成

将取代色满酮(1)与芳肼反应生成的腙与HNCO发生[3+2]环加成反应,加成产物(2)经氧化得到偕偶氮异氰酸酯(3).化合物3在HBF4的催化下发生环化-重排反应,得到新颖的三环系2-氧代-1,2,4-三唑并[3,2-d][1,5]苯并氧氮杂化合物5a～5g.     

Effect of ionic additives on the elution of sodium aryl sulfonates in supercritical fluid chromatography

Addition of a small amount of polar solvent (i.e., modifier) to CO2 in packed column supercritical fluid chromatography (SFC) has shown major improvements in both polar analyte solubility and interaction of the polar analyte with the stationary phase. Recently, the addition of an ionic component (i.e., additive) to the primary modifier by one of us has been shown to extend even further the application of SFC to polar analytes. In this work, the effect of various ionic additives on the elution of ionic compounds, such as sodium 4-dodecylbenzene sulfonate and sodium 4-octylbenene sulfonate, has been studied. The additives were lithium acetate, ammonium acetate, tetramethylammonium acetate, tetrabutylammonium acetate, and ammonium chloride dissolved in methanol. Three stationary phases with different degrees of deactivation were considered: conventional cyanopropyl, deltabond cyanopropyl, and bare silica. The effect of additive concentration and additive functionality on analyte retention was investigated. Sodium 4-dodecylbenzene sulfonate was successfully eluted using all the additives with good peak shape under isocratic/isobaric/isothermal conditions. Different additives, however, yielded different retention times and in some cases different peak shapes.     

烯烃的有机催化不对称环氧化反应

介绍了用手性酮，手性亚胺盐为催化剂以及手性胺为催化剂前体的新型有机催化不对称环氧化反应。     

Direct electrochemistry and enzymatic activity of hemoglobin in positively charged colloid Au nanoparticles and hemoglobin layer-by-layer self-assembly films

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.     

Strategies for multi-site GLP studies

 A GLP study can be performed at more than one site. This is called a multi-site study. Although, the study is performed at different sites, it is still one study and must completely comply with the GLP principles. The fact that different activities are conducted at different sites implies that the planning, the organization and the communication are crucial for the success of the study. This means that all the staff involved should know their responsibilities and should have the knowledge and skills to realize all the phases of the study according to the GLP principles. To achieve a well managed multi-site study, several strategies for setting up such a study can be followed. This paper focuses on the responsibilities, communication, and collaboration of the personnel, which are involved in a multi-site study. Several case studies are highlighted, and we concluded that the basic communication triangle in a single-site GLP study between test facility management, study director, and the quality assurance unit should be extended to the communication among test facility and test site management, study director, principle investigator(s), and the quality assurance units at the test sites. Introduction Received: 14 August 2002 Accepted: 26 November 2002     

Electrocatalytic activity of binary Palladium Ruthenium anode catalyst on Ni-support for ethanol alkaline fuel cells

In search for a cheaper anode catalyst for the oxidation of ethanol for development of direct alcohol fuel cells, Pd has been considered here as an interesting substitute for Pt in Pt Ru binary electrodeposite. The binary catalyst when co-deposited on nickel support has been found to increase the current density and decrease the anodic overvoltage significantly with respect to pure Pt, Pd and Ni. Its electrocatalytic capability is also comparable with that of the Pt-Ru binary electrocatalyst on Ni-support, when studied in 1 M EtOH containing 1 M NaOH solution. The effect of loading of Pd Ru electrocatalyst on Ni support has also been tested. The electrocatalytic activity of the electrodes for oxidation of ethanol has been explained by studies of cyclic voltammetry, chronopotentiometry, steady-state polarization, and conjugated scanning electron microscopy–energy dispersion X-ray spectroscopy. It has been found that electrode containing the higher amount of deposit are less affected by carbonaceous poisons.     

Condensation of 4-aryl-4-oxobutanoic acids with benzylamines: Synthetic and structural studies on 1-arylmethyl-3-[(<Emphasis Type="Italic">E</Emphasis>)-1-arylmethylidene]-5-phenyl-2,3-dihydro-1H-2-pyrrolones

The microwave-mediated reaction of 4-aryl-4-oxobutanoic acids with benzylamines furnished 1-arylmethyl-3-[(E)-1-arylmethylidene]-5-phenyl-2,3-dihydro-1H-pyrrolones. This result is in contract to the earlier report on this reaction conducted under neat conditions. Structures for the products were assigned on the basis of spectral data and confirmed by independent synthesis. __________ Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 368–373, March, 2007.     

通过密度函数理论表征炭质吸附剂的孔径分布

通过密度函数理论（DFT-DensityFunctionalTheory）对炭质吸附剂的孔径分布进行了表征。该法以多孔固体上N2吸附分子模型为依据，用一种方法对多孔固体的孔径分布从微孔到大孔范围进行确定。本文用该法对自制的聚丙烯腈活性炭纤维、国产煤质活性炭及日本产活性炭微球等六种炭质吸附剂的孔径分布进行了表征。     

A new isoprenyl phenyl ether compound from mangrove fungus

A new isoprenyl phenyl ether, 3-hydroxy-4-(3-methylbut-2-enyloxy)benzoic acid methyl ester (1), together with 4-hydroxybenzoic acid (2), 2-hydroxy-6-methylbenzoic acid (3), and 4-hydroxy-3-methoxybenzoic acid (4) were isolated from Mangrove fungus (No. B60) from the South China Sea. The structures of the compounds were established on the basis of NMR spectroscopic and mass spectrometric data. In the preliminary bioassay, compound 1 exhibited antibacterial and antifungal activities. Compound 1 also inhibited cytotoxicity to the hepG2 cell line with an IC₅₀ value of 10.0 μg/mL. Published in Khimiya Prirodnykh Soedinenii, No. 4, pp. 313–314, July–August, 2007.     

Global Forcing Number of Benzenoid Graphs

A global forcing set in a simple connected graph G with a perfect matching is any subset S of E(G) such that the restriction of the characteristic function of perfect matchings of G on S is an injection. The number of edges in a global forcing set of the smallest cardinality is called the global forcing number of G. In this paper we prove several results concerning global forcing sets and numbers of benzenoid graphs. In particular, we prove that all catacondensed benzenoids and catafused coronoids with n hexagons have the global forcing number equal to n, and that for pericondensed benzenoids the global forcing number is always strictly smaller than the number of hexagons.