Ring-chain tautomerism of substituted hydrazones

The freshly distilled products of the reaction of acetaldehyde with 2-(N-propylhydrazino)- and 2-(N-isopropylhydrazino)ethanols have substituted perhydro-1,3,4-oxadiazine structures and are isomerized to the corresponding N-alkyl-N-(2-hydroxyethyl)hydrazones via an equilibrium. Mixtures of both tautomeric forms were isolated by the reaction of these hydrazino alcohols with acetone and pinacolone.See [1] for communication II.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 9, pp. 1167–1170, September, 1971.     

Synthesis and reactions of β-(5-halo-3-uracyl) propionic acids

The reaction of elementary bromine and iodine with -(3-uracyl)-propionic acid has given the corresponding -(5-bromo-3-uracyl) and -(5-iodo-3-uracyl)propionic acids. The methyl esters and amides of the acids have also been synthesized for the first time.     

Synthese de s-triazolo[4,3-d] et [1,5-d] triazines-1,2,4

2-substituted s-triazolo[1,5-d] and 3-substituted s-triazolo [4,3-d]-1,2-4-triazine 8-ones were obtained starting from 5-(3)-alkyl-3(5)-carboxyhydrazino-1,2,4 triazoles and ethyl orthoformate. However, the same reaction was not found to be an efficient one in the case of 5(3)-β-D-ribofuranosyl-3(5)-carboxyhydrazino-1,2,4 triazole.     

519—Reduction of hydrophobic porphyrin at the octane/water interface controlled by the specific adsorption of halogen anions

The redox reaction between the ferric complex of hydrophobic porphyrin and sodium dithionite in two different phases occurring at the interface between two immiscible liquids has been investigated by Volta potential measurements and spectroscopy. The reduction of the ferric complex of hydrophobic porphyrin adsorbed at the interface was found to be accompanied by a potential shift in the negative direction and to depend significantly on the nature of the anion and the ionic strength of the supporting electrolyte. Specifically adsorbed halogen anions inhibited the redox reaction in the sequence: Cl^?, Br^?, I^?. Depending on pH, the ferric complex of hydrophobic porphyrin exists in the uncharged (FeP-O-PFe) form or in the cation FeP⁺ form. The interaction between the ferric complex hydrophobic porphyrin and water has also been investigated.     

Reproducibility of glass open tubular columns in a production environment — Two years of experience

Summary The problems associated with the preparation of glass open tubular (capillary) columns are well documented in the literature. These problems are even more evident if column production is done on a routine basis, in a production environment. On the other hand, from the point of the user who wants to rely on a supplier, the reproducible quality of the columns is crucial. Here quality does not only mean efficiency but also refers to the reproducibility of the average liquid film thickness (capacity ratio) and the relative retention, as well as the tube treatment influencing the polarity of the column tube. In a paper published one year ago [1] our investigation concerning the reproducibility of the column manufacturing process was reported. The present paper continues this investigation. Four different columns will be considered: two types of OV-101 columns with thin and thick liquid film as well as columns prepared with Carbowax 20M and DEGS liquid phases. The consistency of their characteristics and efficiency will be investigated. Column characteristics include the capacity ratio which is directly related to the thickness of the liquid phase film. Column efficiency is investigated with help of the HETP and peak resolution. The effective and theoretical plate numbers are compared and the incorrectness of the assumption that the former is better suited for column testing is demonstrated. Relative retention reproducibility of even difficult peak pairs shows the consistency of column wall treatment. Finally, the consistency and performance of shorter columns obtained by the breaking of long columns will be discussed.Paper presented at the Second International Symposium on Glass Capillary Chromatography, Hindelang, Allgäu, Federal Republic of Germany, May 2–6, 1977.     

Pyridazines. LXV. Reactions of some I-phenacylazolopyridazinium halides with 2,3-diphenylcyclopropenone, -thione,or hydrazine

I-Phenacylazolopyridazinium bromides reacted with 2,3-diphenylcyclopropenone or -thione in the presence of triethylaminc to give 3,4,6-triphenyl-2-pyrone or -2-thiopyrone and the corresponding azolopyridazine. Quaternized azolopyridazines reacted with hydrazine to give either 3,6-diphenylpyridazine and the corresponding azoloazine or hy ring opening of the azine part to give 1-methyl-2-(pyrazolyl-5′)imidazole.     

Polymethylene dyes derived from heterocyclic bases containing condensed thiophene rings

Some new polymethine dyes of the cyanine and merocyanine series which are derivatives of 5- and 6- thienopyridines are synthesized. Replacement of a vinyl group at a sulfur atom in the condensed benzene ring of quinoline in dyes which are derivatives of this base, always leads to a bathochromic shift of the absorption maximum of the corresponding dyes.     

Potassium addition to Fe/MgO, Ni/MgO and Ni/SiO2: Reducibility, dispersity and stabilization of the promoter by the support

The influence of potassium addition on the morphological properties of Fe/MgO and Ni/MgO has been investigated: KNO₃ addition to precursors results in a decrease of the reducibility and in a smaller dispersity of the metallic phase. A loss of potassium is observed at reduction temperatures in excess of 773 K. Silica-supported Ni behaves differently: silica inhibits the potassium volatilization and nickel reducibility is enhanced. This illustrates how promoter effects can be influenced by the nature of support.

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Fe/MgO Ni/MgO: KNO₃ . , 773 K. , : . .

     

Spectrophotometric determination of nickel(II) in different samples by complexation with some triazolylazo dyes

A new sensitive spectrophotometric method for the determination of nickel(II) with 3-(2-hydroxy-5-acetyl-(L¹),-5-ethoxycarbonyl-(L²),-5-methyl-(L³),-5-formyl-(L⁴),-5-bromophen-1-ylazo)-1,2,4-triazole (L⁵), and 3-(2,4-dihydroxyphen-1-ylazo)-1,2,4-triazole (L⁶) in aqueous media containing 40 vol. % methanol has been developed. The method is based on the formation of stable coloured Ni(II) complexes with stoichiometric ratios 1: 1 and 1: 2 (n(M): n(L)). Linear calibration graphs are obtained up to 7.04 μg cm⁻³ of nickel(II) under optimum conditions attained from investigation of complex formation. The absorption maxima varied from 485 nm to 545 nm and the molar absorptivities ranged from 0.84 × 10⁴ to 4.65 × 10⁴ dm³ mol⁻¹ cm⁻¹ for 1: 1 and 1: 2 (n(M): n(L)) complexes with varying the substituent on the phenolic ring. The optimum ranges for the direct determination of nickel(II) (Ringbom) and the stability constants of the formed complexes are determined. The developed method was applied to the spectrophotometric determination of nickel(II) in some samples with satisfactory results.     

Organic phase conversion of bulk (wurtzite) ZnO to nanophase (wurtzite and zinc blende) ZnO

We describe the all-organic phase conversion of bulk commercial ZnO in the wurtzite modification to sub-30 nm ZnO that we find to be partially in the zinc blende [, a=4.568(3) Å] modification. The conversion involves refluxing ZnO in 2,4-pentanedione (acetylacetone) at 413 K to form the zinc 2,4-pentanedionate, which is decomposed by heating at 573 K in an appropriate high-temperature solvent such as dibenzylether to form nanophase ZnO. This nanophase, partially zinc blende ZnO can also be obtained in a single step by heating commercial zinc 2,4-pentanedionate in refluxing dibenzylether. Thermodiffractometry suggests that the conversion of zinc blende ZnO to wurtzite ZnO commences near 650 K.