Isolation of 2-Chloro-5-methylpyridine from its Isomer 2-Chloro-3-methylpyridine by Formation of its Copper(II) Complex

2-Chloro-5-methylpyridine is an important intermediate for the preparation of biological active compounds, especially insecticides1, e.g. imidacloprid2, and is usually manufac- tured from 3-methylpyridine N-oxide. However, the manufacturing process also forms the by-products: 3-methylpyridine and its isomer 2-chloro-3-methylpyridine3. The pro- perties of the isomers are similar, it is difficult to separate by ordinary methods, such as distillation. Scheme 1 79.4%13.6%5.2%NClCH3NCH3ClNC…     

Trovacenchemie. 13 [1] Weg und Irrweg zu Di([5]trovacenyl)keton

Trovacene Chemistry. 13 [1] On Being Lead and Mislead in the Synthesis of Di([5]trovacenyl)ketone Di([5]trovacenyl)ketone ( 3¨ ) has been prepared from lithio‐[5]trovacene and dimethylcarbamoyl chloride and studied by X‐ray diffraction, cyclic voltammetry, magnetic susceptometry and EPR spectroscopy. Slight variation of the synthetic protocol affords an unusual trinuclear complex 5 ? that is also fully characterized. Spin‐spin exchange interaction is smaller in 3¨ than in 1,1‐di([5]trovacenylethene ( 2¨ ), which differs from 3¨ by a replacement of O for CH₂. The novel trinuclear complex 5 ? , however, displays exchange coupling very similar to that observed in 1‐methoxy‐2,5,6‐tri([5]trovacenyl)benzene ( 7 ? ). In both cases, an unsymmetrical triangular arrangement of S = 1/2 centers is encountered. These findings are discussed in terms of the nature of the respective spacers.     

Study of the spontaneous formation of organic layers on carbon and metal surfaces from diazonium salts

This study investigates the spontaneous grafting of different para-substituted phenyl groups on carbon and metallic surfaces from diazonium salts solutions. Glassy carbon, nickel, zinc and iron plates were allowed to react with an acetonitrile solution of aryldiazonium tetrafluoroborate salt by simple dipping. The surfaces were characterized before and after their immersion by XPS and AFM to evidence the formation of a coating on the different materials. The results are indicative of the presence of substituted phenyl groups on all the investigated surfaces. This study also aims at correlating grafting efficiency with metal reactivities and diazonium salt electronic properties by means of AFM and FT-IRRAS. For this purpose, zinc and nickel were chosen due to their opposite reducing properties and two diazonium salts were selected with electron-donor or -withdrawing para-substituents. The results tend to indicate that redox properties of both partners (diazonium + metal) are of prime importance for grafting to occur.     

乙酰丙酮稀土四苯基卟啉配合物的电化学研究

本文指出我国环境保护产业发展中存在的问题，论述了“入关“对我国环境保护产业的影响及应采取的经济和税收政策。     

Simultaneous isolation and determination of esculin and rutin in natural materials using SPE and HPLC

Summary Esculin (ESC) and rutin (RUT) have been simultaneously isolated from pharmaceutical natural materials by solid phase extraction (SPE). Determination of both substances was performed by reversed phase high performance liquid chromatography (RPHPLC) with UV detection. Optimization of the separation conditions showed that simultaneous isolation and determination of rutin and esculin from pharmaceutical material was possible. The recovery obtained was not lower than 95±2%.     

ORGANIC CHELATING REAGENT ON REDOX ADSORPTION OF ACTIVATED CARBON FIBER TOWARDS Au^3+

Organic chelating reagent influences upon the redox adsorption of activated carbon fibertowards Au3- were systematically investigated. The experimental results indicated that the presenceof organic chelating reagent on activated carbon fiber strongly affects adsorption capacity ofactivated carbon fiber towards Au3+. The reduction-adsorption amount of Au3+ increased three timesby the presence of 8-quinolinol. Furthermore, The reduction-adsorption amount of Au3+ depended onthe pH value of adsorption and temperature.     

Validation of the thermodynamic model of inorganic arsenic in non polluted river waters of the Basque country (Spain)

The thermodynamic model of inorganic arsenic was validated by comparing the predicted As(III) concentration with the experimentally determined one in several river waters samples of the Basque Country (Spain) collected in two sampling campaigns: spring and autumn 2000. This model takes into account the acid-base equilibria of As(III) and As(V) together with the redox equilibria between the H₃AsO₃ and H₃AsO₄ species. A correct prediction of As(III) concentration requires the knowledge of the total concentration of arsenic, pH, redox potential (referred to hydrogen electrode), and ionic strength values of the solution. The estimation of the activity coefficients of the arsenic species was performed by means of the Modified Bromley’s Methodology (MBM).In order to perform the experimental As(III) determination, an analytical method was implemented by using an ion exchange separation of As(III)/As(V) on a continuous FIA-IE-HG-AAS system. The total arsenic concentration was determined together with total concentration of the main alkaline or alkaline-earth metals and anions in the natural waters. Temperature compensated measurements of the pH and redox potentials were made in-situ at the sampling sites.For both seasonal campaigns, the agreement between predicted and experimental As(III) is really high for those samples belonging to non polluted river waters.     

含吡咯烷酮基丙烯酸酯类单体的合成及聚合

轻度交联的聚甲基丙烯酸2-羟乙酯(HEMA)是众所周知的医用水凝胶,即所谓的“Hvdron”。但其吸水率一般在59%(EWC为37%),并不尽人意。近年来,为了提高这类水凝胶的亲水性及生物相容性,常用一些亲水性的烯类单体进行表面改性或通过共聚以达到此目的,N-乙烯基吡咯烷酮是较为常用的这类单体之一。本文合成了含吡咯烷酮基丙烯酸酯类的单体,即丙烯酸2-N-吡咯烷酮基乙酯(PyEA),甲基丙烯酸2-N-吡咯烷酮基乙醋(PyEMA),并研究了这两种单体在甲基丙烯酸二甲氨乙酯(DMAEMA)与过硫酸钾(KPS)所组成的氧化还原引发体系下的聚合。     

一种新型织绵芋螺毒素可增强神经元钙电流

从中国南海织绵芋螺中分离出生物活性强、电生理效应特异的新的芋螺毒素。通过毒素分离纯化,并经生物活性测定,氨基酸测序,电生理效应等研究。分离到1种新的织绵芋螺毒素Tx7,它是由27个氨基酸组成。其序列为GCSSVCNSHTDCVTHCICTFRGCGAVN,并能引起小鼠痉挛,能增强海马神经元钙电流和提高兴奋性突触后电流的发放频率。实验表明Tx7具有较高的潜在应用价值。1实验部分1.1材料与仪器织绵芋螺,昆明种小鼠(20±2g),Bio-rad凝胶HPLC柱,BIFLEXⅢ型飞行时间质谱仪,491型蛋白质自动测序仪。     

Three-way-output response system by electric potential: UV-vis, CD, and fluorescence spectral changes upon electrolysis of the chiral ester of tetracyanoanthraquinodimethane

The newly prepared tetracyanoanthraquinodimethane (TCNAQ) derivatives 1a,b with a chiral auxiliary are good electron acceptors and exhibit weak circular dichroism (CD) based on the absorption of TCNAQ. The twin-type electron acceptor 1c with two TCNAQ units shows larger ellipticity by exciton coupling. UV-vis, CD, and fluorescence spectra were changed drastically upon electrochemical reduction of 1c, which demonstrates the unprecedented three-way-output response system.