Cyclization of n-alkylazinium cations with bisnucleophiles. 4. Regio- and stereospecificity of the reactions of β-diketones with quinoxalinium salts and their aza and benzo analogs

The reactions of substituted quinoxalinium, benzo[g]- and benzo[f]quinoxalinium, and pyrido[2,3-b]pyrazinium salts with anions of -dicarbonyl compounds give furo[2,3-b]-annelated systems with strictly determined regio- and stereoorientations.See [1] for Communication 3.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 11, pp. 1543–1548, November, 1981.     

Mesoionic 1-amino-1,3,4-triazole-2-thiones and their azomethine derivatives

The reaction of triethylammonium salts of -acyldithiocarbazic acids with sodium chloroacetate and hydrazine leads to the formation of mesoionic 1-amino-1,3,4-triazole-2-thiones, which react with aldehydes to give the corresponding azomethine derivatives.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 424–428, March, 1976.     

Steric structure of phosphorus-contaiming heterocycles

Conclusions The steric structure of 3-halo-1-thia-3-phosphethanes with a tetracoordinated phosphorus atom was investigated by the methods of dipole moments and Kerr constants, enlisting data on quantum chemical calculations of the energies of the conformations.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 10, pp. 2240–2244, October, 1973.The authors would like to thank I. M. Shermergorn for providing the samples for the investigations.     

Friedel-crafts copolymerization of thiophene and p-di(chloromethyl)benzene. II. Products of the later stages of the reaction

Products of the copolymerization of thiophene and p-di(coloromethyl)benzene in presence of stannic chloride have been separated by using gel-permeation chromatography (GPC) and identified by using principally mass, infrared, and nuclear magnetic resonance spectroscopy. The GPC separation is not nearly as efficient as the separation of the products of the corresponding benzene–DCMB and diphenylmethane–DCMB reactions which have previously been described. A further complication which makes a kinetic analysis of this reaction more difficult is the occurrence of intramolecular condensation of certain of the earlier products leading to cyclic structures incorporating four aromatic rings. These investigations have made it possible to deduce some of the principal structural differences between the thiophene–DCMB and benzene–DCMB polymers which may have some bearing on the differences which have been found in their thermal stabilities.     

EDXRF as an analytical tool in art: Case studies from pigment identification and treatment assessment

Energy dispersive X-ray fluorescence (EDXRF) was employed for the identification of pigments decorating Hellenistic figurines, and the assessment of the efficiency of a treatment with barium hydroxide applied to stone. Elements present in the colored areas of the figurines, as well as the treated stone was identified by EDXRF. These data together with complementary information obtained by Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction analysis (XRD) led to the identification of several precious pigments. As far as the treatment efficiency is concerned, EDXRF analysis revealed that barium is unevenly distributed on the treated surface and reaches a maximum depth of 2.5 mm.     

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.     

Properties and structures of porphyrexides

The molecular and crystal structures of porphyrexides, viz., 4-amino-2-imino-(1) and (Z)-2-amino-4-bromoimino-5,5-dimethyl-4,5-dihydro-1H-imidazole 1-oxyls (7), and their diamagnetic precursors were determined. Compound 1 is kinetically unstable because it is oxidized with atmospheric oxygen to form (E)-1,2-bis[1-amino-1-(cyanoimino)-2-methyl-propan-2-yl]diazene 1,2-dioxide. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 441–447, March, 2006.     

Heterometallic nickel(II) samarium(III) diethylenetriaminepentaacetate, a starting material for the preparation of samarium nickelate films

A reaction of samarium oxide, nickel oxocarbonate, and diethylenetriaminepentaacetic acid (H₅DTPA) taken in stoichiometric proportions in water gave SmNiDTPA · 10H₂O as a glassy solid. The formation of this heterometallic complex was confirmed by data from elemental analysis, IR spectroscopy, thermal analysis, and X-ray fluorescence analysis. An aqueous solution of the complex was used to deposit SmNiO₃ films onto a single-crystal SrTiO₃(001) substrate. The SmNiO₃ phase in films obtained upon 3-h annealing at 500°C was identified by powder X-ray diffraction. Films deposited from a solution of an equimolar mixture of monometallic samarium and nickel diethylenetriaminepentaacetates contained no samarium nickelate.