ω-(2-benzimidazolyl)perfluorinated carboxylic acids and their derivatives

A convenient method is proposed for the preparation of -(2-benzimidazolyl) perfluorinated carboxylic acids and their amides by condensation of o-phenylenediamine with imides of perfluorinated dicarboxylic acids. The transformations of the o-aminoanilides of the amides of the perfluorinated dicarboxylic acids were studied by thermal analysis and mass spectroscopy.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1262–1265, September, 1976.     

Voltammetric studies of the Kolbe synthesis with perfluorocarboxylic acids prepared from hexafluoropropene oxide oligomers

Carboxylic acids prepared from hexafluoropropene oxide CF₃CF₂CF₂O[CF(CF₃)CF₂O]_nCF (CF₃)COOH [n = 0, 2,5-bis(trifluoromethyl)-3,6-dioxaperfluorononanoic acid; n = 1, 2,5,8- tris(trifluoromethyl)-3,6,9-trioxaperfluorododecanoic acid], according to voltammetric data, enter the Kolbe reaction both at the Pt anode and at anodes from carbon materials in H₂O-CH₃CN and CH₃OH-CH₃CN solutions. The critical potential appreciably depends both on the anode material and on the solvent composition. Favorable effect of pyridine additions in H₂O-CH₃CN solutions is due to replacement of water molecules from the electrical double layer. The sodium ions exert a negative effect on the Kolbe synthesis.Translated from Zhurnal Obshchei Khimii, Vol. 74, No. 11, 2004, pp. 1842–1846.Original Russian Text Copyright © 2004 by Chechina, Sokolov, Tomilov.This revised version was published online in April 2005 with a corrected cover date.     

Synthesis of Nitroesters Based on Methylol Derivatives of Parabanic and Isocyanuric Acids

Nitroesters synthesis based on methylol derivatives of parabanic and cyanuric acids was performed. The corresponding alloxan nitroxymethyl derivative was unstable.__________Translated from Zhurnal Organicheskoi Khimii, Vol. 41, No. 2, 2005, pp. 264–265.Original Russian Text Copyright © 2005 by Ermakov, Bulatov, Vinogradov, Tartakovskii.     

Localization of electrochemically generated radicals as a function of their structure and the nature of the solvent

The electrooxidation of different perfluorocarboxylic acids has been investigated in the presence of ethylene, on electrodes with different adsorbing power [platinum and glassy carbon (GC)] in different solvents. It has been shown that the reaction zone of the ECG radicals is determined by their solubility; depending on this, it can be limited to the electrode surface or encompass the entire volume of the solution. The concept of the solubility of the ECG radicals made it possible to establish some regularities in the formation of cross combination products in the Kolbe electrosynthesis of different perfluorocarboxylic acids.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 5, pp. 1134–1141, May, 1991.     

Anodic perfluoroalkylation of the enol acetate of ethyl acetoacetate

Electrochemical perfluoroalkylation of the enol acetate of ethyl acetoacetate was studied in the conditions of the Kolbe reaction. The yields of alkylation products depend on the competing adsorption of the enol acetate, the solvent, and perfluorocarboxylates on the surface of a platinum electrode.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2948–2951, December, 1996.     

Competitive Formation of β-Amino Acids,Propenoic, and Ylidenemalonic Acids by the Rodionov Reaction from Malonic Acid,Aldehydes, and Ammonium Acetate in Alcoholic Medium

The Rodionov reaction of 49 available aliphatic and aromatic aldehydes with malonic acid and ammonium acetate in alcoholic medium, resulting in formation of β-amino acids, propenoic, and ylidenemalonic acids, was studied. Certain regioselectivity regularities of the reaction were revealed. Among the variety of ketones studied, cyclohexanone is the only whose reaction yields a β-amino acid. Unusual dehydrofluorination of 6-chloro-2-fluorocinnamic acid under the Rodionov reaction was discovered.__________Translated from Zhurnal Obshchei Khimii, Vol. 75, No. 7, 2005, pp. 1177–1186.Original Russian Text Copyright © 2005 by Lebedev, Lebedeva, Sheludyakov, Kovaleva, Ustinova, Kozhevnikov.     

Synthesis of thieno[3.2-<Emphasis Type="Italic">b</Emphasis>]pyrrolenine derivatives under the Fischer reaction conditions

The reaction of alkyl 4-(2-acetylhydrazino)-2-methyl-3-thiophenecarboxylates with 3-methylbutan-2-one was carried out under the Fischer reaction conditions. The influence of Lewis acids and solvents on the process was studied. A convenient method for the synthesis of thieno [3.2-b]pyrrolenine derivatives was proposed.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 725–729, March, 2005.     

Synthesis and Properties of Some New Nicotinoyl Isocyanates and Their Fragmentation under Electron Impact

A convenient preparative route for synthesis has been developed and nicotinoyl isocyanates (NIC) have been obtained for the first time by the action of oxalyl chloride on amides of substituted nicotinic acids. A procedure has been found for suppressing the formation of hydrochlorides of nicotinoyl amides by the competing reaction of HCl with the initial amides of nicotinic acids. The special features of the fragmentation of nicotinoyl isocyanates under electron impact have been studied.__________Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 549–553, April, 2005.     

Adsorption of Aliphatic Acids from Aqueous Solutions at the Interface with the Gas Phase

The type of the dependence of the Gibbs relative adsorption on the concentration of an ideal solution of a surfactant was studied. The applicability of the hypothesis of monomolecular adsorption at the interface between an aqueous solution of aliphatic acids and the gas phase was assessed.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 5, 2005, pp. 747–750.Original Russian Text Copyright © 2005 by Malov.     

Synthesis and characterization of novel perfluorinated polyimides with 3D‐controlled structures for photonic applications

We have designed and synthesized novel perfluorinated polyimides with 3D controlled structure. At first, we successfully developed the new synthetic routes to diamines with pendant bulky perfluorinated aromatic units in a multi‐step synthetic procedure. Novel perfluorinated polyimides were prepared in a two‐step reaction in N‐methyl‐2‐pyrrolidinone (NMP) solution: The first step was for the synthesis of polyamic acids (PAAs) and the second reaction was for the imidization of PAA. The polymer yield was over 89% and the inherent viscosity of PAAs was in the range of 0.24–0.36 dL/g. The thin films were prepared by spin‐coating the PAA solution in NMP onto various substrates such as a Si wafer or a KBr pellet, dried at 80 °C and further cured at 230 °C. The resultant polyimides are thermally stable over 400 °C. The refractive index and birefringence of the resultant polyimides are 1.5858–1.6452 and 0.01–0.005, respectively. The refractive index of polyimide decreases with increasing the fluorine content. The copolymerization and the ether linkages into the backbone reduce the birefringence of polyimides. Surprisingly, the pendant ether linkage is not a crucial factor in reducing the polyimide birefringence. Their birefringence is comparatively very low, compared with that of previous polyimides. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 1326–1342, 2006     

Synthesis of Metallofullerenes by Electric-Arc Method with a Surface-Modified Electrode

A method for synthesis of metallofullerenes by electric-arc sputtering of graphite, in which lanthanum compounds are deposited on the surface of a graphite electrode, was suggested. The influence exerted by the amount of deposited lanthanum on the yield of lanthanum was studied.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 4, 2005, pp. 566–571.Original Russian Text Copyright © 2005 by Kuz’min, Borovkov, Kolker, Brazhyunas.     

Synthesis of Dispersed System (CuO,ZnO) from Lump Braze with a Vertical Flow-through Electrolyzer

The electrochemical synthesis of a mixture of dispersed oxides (CuO and ZnO) from secondary lump braze was studied. The influence exerted by electrolysis parameters on the intensity of synthesis of the oxide mixture was investigated. The design of the electrolyzer and the flow diagram for synthesis of a mixture of oxides (CuO and ZnO) from lump braze was suggested.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 2, 2005, pp. 249–252.Original Russian Text Copyright © 2005 by Kuntyi, Olinets, Kalymon, Olenych.     

Formation of silver clusters by borohydride reduction of AgNO<Subscript>3</Subscript> in polyacrylate aqueous solutions

Chemical synthesis of the compounds of silver clusters and polyacrylate was performed using sodium borohydride as a metal cation reducing agent. The effect of silver cation content on spectral properties and structure of the synthesized metal—polymer systems was studied by optical spectroscopy and transmission electron microscopy.Translated from Kolloidnyi Zhurnal, Vol. 67, No. 1, 2005, pp. 79–86.Original Russian Text Copyright © 2005 by B. Sergeev, Lopatina, Prusov, G. Sergeev.     

Synthesis of 3-(3″-Aminobenzoylamido)-1-(2′,4′,6′-trichlorophenyl)pyrazol-5-one,an Intermediate in the Synthesis of the Purple Component of Color Photographic Materials

Catalytic reduction of 3-(3″-nitrobenzoylamido)-1-(2′,4′,6′-trichlorophenyl)pyrazol-5-one with hydrogen and hydrazine hydrate to 3-(3″-aminobenzoylamido)-1-(2′,4′,6′-trichlorophenyl)pyrazol-5-one, the key intermediate in the synthesis of the purple component of color photographic and motion-picture materials, was studied.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 2, 2005, pp. 284–286.Original Russian Text Copyright © 2005 by Yutilov, Smolyar, Minkina.     

Pseudo-Topochemical Synthesis of α-Fe in Aqueous Solution Using an Aluminum Matrix

Processes occurring in synthesis of α-Fe from a Fe(III) solution using an aluminum matrix were studied. The reaction kinetics strongly depends on the state of the matrix.__________Translated from Zhurnal Obshchei Khimii, Vol. 75, No. 2, 2005, pp. 177–183.Original Russian Text Copyright © 2005 by Dresvyannikov, Kolpakov.     

Preconcentration of Cadmium with OP-10 Nonionic Surfactant Phases at the Cloud Point

The effect of the main parameters on the extraction of cadmium with carboxylic acids into the micellar phase of the OP-10 nonionic surfactant at the cloud point was studied. Conditions were found for the atomic absorption determination of cadmium in natural and waste waters using the micellar-extraction preconcentration with capric acid and n-octylamine into the surfactant phase.__________Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 5, 2005, pp. 458–462.Original Russian Text Copyright © 2005 by Doroshchuk, Kulichenko.     

Electrokinetic Phenomena in Sulfonated Cation-Exchange Membranes with Tetraalkylammonium Ions

The electric transport of solvent ions and molecules through membrane systems containing cations of tetraalkylammonium bases is studied. The interrelation between electrokinetic characteristics of sulfonated cation-exchange membranes at different degrees of their saturation with tetrabutylammonium ions and the content of water in membranes at equilibrium is established. A new type of conductor-insulator percolation transitions is revealed for homogeneous MF-4SK perfluorinated membranes saturated with organic counterions. This transition is interpreted with allowance for the concept of the governing role of narrow channels in the membrane microstructure. The electroosmotic permeability of MF-4SK membranes in solutions of sodium and tetraethylammonium chloride, as well as in their mixtures, is studied. An experimentally observed abnormally high amount of water transferred by tetraethylammonium ions is discussed with allowance for the dynamic hydration characteristics of ions.__________Translated from Kolloidnyi Zhurnal, Vol. 67, No. 4, 2005, pp. 485–493.Original Russian Text Copyright © 2005 by Kononenko, Berezina, Shkirskaya.     

A Study of the Kinetics of Synthesis of Potassium Superoxide from an Alkaline Solution of Hydrogen Peroxide

Kinetic aspects and the mechanism of shaping of particles of potassium superoxide in its synthesis from drops of an alkaline solution of hydrogen peroxide in a flow of a drying agent were studied.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 2, 2005, pp. 191–194.Original Russian Text Copyright © 2005 by Zhdanov, Ul’yanova, Ferapontov.     

Kolbe carbon-carbon coupling electrosynthesis using solid-supported bases

We have developed a novel electrolytic system for Kolbe carbon-carbon coupling electrosynthesis based on the acid-base reaction between carboxylic acids as a substrate and solid-supported bases. On the basis of the electrolytic system, Kolbe electrolysis of various carboxylic acids was successfully carried out to provide the corresponding homocoupling products in moderate to excellent yields.     

Extraction of Aromatic Sulfonic Acids in the Presence of a Surfactant

Extraction of phenol- and naphtholsulfonic acids from aqueous salt solutions in the presence of a surfactant, N-cetylpyridinium chloride, with hexane, ethylbenzene, and acetone-diacetone alcohol is studied.__________Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 1, 2005, pp. 79–82.Original Russian Text Copyright © 2005 by Korenman, Gubin, Sukhanov.