Chemical properties of ylidene derivatives of azines. 3. Synthesis and reactions of ylidene derivatives of halopyrimidines

Some dihydropyrimidines have been obtained which contain a cyanoacetic ester or malononitrile residue and chlorine in positions, 2, 4, and 6. The reactions of these compounds with nucleophiles has been examined.For communication 2, see [1].Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 7, pp. 963–969, July, 1986.     

Reactions of 1,2,4-Triazines with Nucleophiles. 6. Use of SNH Methodology for the Direct Introduction of Cyclic Diketone Residue into the 1,2,4-Triazine Ring FORENAME = D. N.

3-R-6-Phenyl-1,2,4-triazine 4-oxides react with cyclic -diketones (dimethylbarbituric acid, dimedone, and indan) in both acidic (substrate activation) and basic conditions (nucleophile activation) with formation of ^H-adducts, intermediates in the nucleophilic substitution of hydrogen (S_N ^H) in 3-R-5-Nu-4-hydroxy-6-phenyl-4,5-dihydro-1,2,4-triazines. Oxidative aromatisation of these intermediates or auto-aromatisation of acylated (benzoyl chloride) at the NOH -adducts with elimination of benzoic acid gave the corresponding substituted 1,2,4-triazine 4-oxides or 1,2,4-triazines.     

Analysis of the terphenyls by a compressed pellet infrared method involving micro-distillation

A quantitative compressed pellet infrared method used together with a micro-distillation to effect separation of the isomer has been developed and reported here for the analysis of ortho-, meta-, and para-terphonyl. The terphenyl content is determined on fractions isolated by distillation from radiation damaged samples. The compressed pellet infrared method is preferred instead of the more conventional solution technique since smaller quantities of isolated terphcnyl are required. The pellet method is applicable also to polyphenyls higher than the terphenyls. The solution technique is not due to the insolubility of the polyphenyls. It is expected that the compressed pellet spectral method developed here might well find application in the analysis of compounds other than polyphenyls. Results presented here appear to be the, first quantitative infrared data reported in the literaturu on polyphenyl compounds.     

Electrochemical Hydrogenation of Substituted α-Phenylvinylphosphonic Acids: General Characteristics of the Reaction Layer and Prediction of Preparative Electrolysis Conditions

The conditions for electrochemical hydrogenation and anodic oxidation of -phenylvinylphosphonic acid and its 4-chloro- and 4-methyl-substituted derivatives on palladized platinum electrodes in aqueous sulfuric-acid solutions are found. It is shown that, in the system under study, the products of strong chemisorption are not the intermediates of the electrocatalytic hydrogenation. The reactant molecules are modeled by quantum-chemical methods in terms of the restricted Hartree–Fock approximation. The calculated charge distributions in reactant molecules are used for estimating the electrostatic components of works of approach and the orientation distributions in the reaction layer.     

Analysis of 19-norandrosterone in human urine by gas chromatography–isotope-dilution mass spectrometry: method adopted by LGC for participation in the Comité Consultatif pour la Quantité de Matière (CCQM) Pilot Study P68

The method used at LGC for analysis of “total” 19-norandrosterone (19-norandrosterone glucuronide plus “free” 19-norandrosterone) in urine for the Comité Consultatif pour la Quantité de Matière Pilot Study (CCQM-P68) is described. The analytical method used was a modified version of the method developed at the National Measurement Institute of Australia, which used a hydrolysis and derivatisation procedure first described by the German Sports University. This method is routinely used by World Anti-Doping Agency-accredited laboratories for sports drug testing. The main modifications made to the method were the use of 19-norandrosterone glucuronide as a calibration standard and 19-norandrosterone glucuronide-d4 as an isotopically labelled internal standard, and the use of a bench-top quadrupole gas chromatograph–mass spectrometer. The results produced by LGC (2.14 ± 0.15 ng g⁻¹ expanded uncertainty, coverage factor k = 2) were in excellent agreement with those from other participating national metrology institutes and thus further validates the exact-matching isotope-dilution mass spectrometric procedures used at LGC for a wide range of reference measurement applications, including measurement of ng g⁻¹ levels of steroids in a biological matrix.     

Quantum-Chemical Study of Proton Transfer and Photoreactions of Quinolone Derivatives

The possible routes of deactivation of electronically excited states of 4-methyl-7-hydroxy-2-quinolone and its protolytic forms were analyzed. The relative contribution of radiative and nonradiative deactivation channels of electronic excitation energy was determined, and the rate constants of photophysical processes (internal conversion and intersystem crossing) occurring upon light absorption by these forms were estimated.     

Furan derivatives of group I elements (review)

Latvian Institute of Organic Synthesis, Riga LV-1006. Translated from Khimiya Geterotsikiicheskikh Soedinenii, No. 4, pp. 435–473, April, 1995. Original article submitted February 22, 1995.     

Kinetics of the thermal desorption of O2, HCl,and H2O from the surface of cobalt chromite

A study has been carried out on the kinetics of the temperature-programmed desorption of O₂, HCl, and H₂O from the surface of cobalt chromite. A mathematic model was obtained for the kinetics of the thermal desorption and a method was developed for determining the kinetic constants. The kinetic parameters of the desorption of O₂, HCl, and H₂O were calculated using these experimental data.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 29, No. 5, pp. 449–455, September–October, 1993.     

Isomerization of S-2-hydroxyalkyl esters of cyclic phosphorus thioacids

Conclusions The S-2-hydroxyalkyl esters of cyclic P(V) thioacids, which were obtained by reacting a cyclic phosphorus monothioacid with an alkylene oxide, are converted to the 2-mercaptoalkyl esters of cyclic phosphorus acids independent of the size of the ring.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 11, pp. 2594–2596, November, 1980.