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Benzathine is prepared in good yields from cyanobenzene by a combination of electrochemical hydrogenation and Kolbe electrolysis using nickel and platinum electrodes in the presence of methanolic sodium methoxide in an undivided cell.  相似文献   

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A synthesis of 6-aminonicotinic acid by electrochemical hydrogenation of 5-chloro-2-nitropyridine and electrochemical carboxylation of 2-amino-5-chloropyridine at a cathode surface in the presence of sulphuric acid and carbon dioxide in a dimethylformamide (DMF) solution at an apparent current density of 10 mA/cm2 using an undivided cell with good yields is reported.  相似文献   

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Electrochemical oxidation of 3,4-dihydroxybenzoic acid (1) in the presence of 1,3-dimethylbarbituric acid (2) and 1,3-diethyl-2-thiobarbituric acid (3) as nucleophiles in aqueous solution has been studied using cyclic voltammetry and controlled-potential coulometry. The results indicate that 1 via Michael reaction under electro-decarboxylation reaction converts to benzofuro[2,3-d]pyrimidine derivatives (6a, 6b). The electrochemical synthesis of 6a, 6b has been successfully performed in an undivided cell in good yields and purity.  相似文献   

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Two-electron reduction of some substituted 1,2-dithiole-3-thiones 1 followed by alkylation of the dianionic intermediates leads through electrosynthesis to mixture of Z and E isomers of the corresponding substituted alkyl-(3-thioalkyl)-2-propenedithioates 2, 3 in satisfactory yield. The structure of those products was established by 13C and 1H nmr and mass spectroscopy. The isomers ratios were determined by nmr spectroscopy.  相似文献   

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Shen Y  Atobe M  Fuchigami T 《Organic letters》2004,6(14):2441-2444
[reaction: see text] Anodic intramolecular cyclization of alpha-(phenylthio)acetamides using a fluoride ion mediator was realized. Under ultrasonic irradiation, cyclization was accelerated markedly to give desired cyclized products in moderate to good yields. The local heating effect of ultrasonic irradiation seems to be more advantageous than usual heating.  相似文献   

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赵萍  尹应武 《有机化学》2003,23(7):628-635
对近年来电辅基在有机电合成中的应用研究概况进行了综述。电辅基共分为两 大类,第一类电辅基是由第四主族的无素参与组成的有机基团,而有机硫基团属于 第二类电辅基。电辅基可以使分子的最高占有轨道(HOMO)的能量升高,促进电子 的传递,从而降低有机底物的氧化电势,使碳原子与电辅基相连化学键选择性地断 裂,同时接受亲核试剂的进攻,使反应的选择性提高。电辅基在今后的有机化学合 成中具有广阔的应用前景。  相似文献   

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Manabu Kuroboshi 《Tetrahedron》2009,65(34):7177-7185
Oil-in-water nanoemulsion which consisted of TEMPO, amphiphilic alcohols, and water offered unique reaction environments for electrooxidation of the alcohols to give the corresponding carboxylic acids in good to excellent yields.  相似文献   

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Electroorganic synthesis is a promising tool to design sustainable transformations and discover new reactivities. However, the added setup complexity caused by electrodes in the system impedes efficient screening of reaction conditions. Herein, we present a microfluidic platform that enables automated high-throughput experimentation (HTE) for electroorganic synthesis at a 15-microliter scale. Two HTE modules are demonstrated: 1) the rapid electrochemical reaction condition screening for a radical–radical cross-coupling reaction on micro-fabricated interdigitated electrodes, and 2) measurements of kinetics for mediated anodic oxidations using the microliter-scale cyclic voltammetry. The presented modular approach could be deployed for a range of other electroorganic chemistry applications beyond the demonstrated functionalities.  相似文献   

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李文辉 《合成化学》2002,10(2):177-179,182
以5-羟甲基糠醛及其加成产物为原料,用化学或电化学合成法合成了标题化合物,其产物结构经元素分析,IR和^1H NMR确证。  相似文献   

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In the electroreduction of sulfonium and ammonium salts, sulfonium ylid was generated from the sulfonium salt, whereas in the case of the ammonium salt, nitrogen ylid was not formed but the N+C bond was reductively cleaved. On the basis of the controlled potential electrolysis, it seems acceptable that the mechanism of formation of sulfonium ylid involves the direct electron transfer to the sulfonium salt as the initiation step.  相似文献   

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The electrochemical formation and regeneration of redox agents for organic syntheses (indirect electrolysis) widens the potential of electrochemistry, as higher or totally different selectivities can often be obtained while at the same time the energy input can be lowered significantly. Higher current densities can also be obtained by preventing otherwise often encountered electrode inhibition. New types of redox catalysts can be formed in-situ and can be regenerated after reaction with the substrates. This principle is of increasing importance also for the application of already known redox agents with regard to environmental protection, since large amounts of a product can be generated in a closed circuit using only relatively small amounts of the redox reagent. Consequently the operation of such a process can be greatly simplified, and the release of ecologically objectionable spent reagents into the environment can be prevented. The broad spectrum of redox catalysts currently in use includes, inter alia, metal salts in very low or high oxidation states, halogens in various oxidation states, and, in particular, a wide variety of transition-metal complexes. A great deal of progress has recently been made in the application of organic electron transfer agents, since compounds have been found that are sufficiently stable in both the reduced as well as the oxidized state.  相似文献   

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