Synthesis and ring-chain isomerism of acid chlorides and amides of 2-(2-pyridyl and 2-quinolylcarbonyl) benzoic acids

The reaction of 2-(2 pyridytcarbonyl)benzoic acid with thionyl chloride affords an unexpected product of the intramolecular acylation of the pyridine nitrogen atom, namely, 6,11-dioxo-6,11-dihydrobenzo[blquinotizinium chloride. At the same time, 2-(2-quinotylcarbonyl)benzoic acid forms the expected cyclic acid chloride, namely, 3-(2-gitinotyl)-3-chlorophthalide in this reaction. Both compounds acylate ammonia and primary amines, including those with bulky alkyl groups (tert-butyl, 1-adamantyl, and 1,1,3,3-tetramethylbutyl) with the formation of 2-R-3-hydroxy-3-(2pyridyl- or 2-quinolyl)isoindolines. The protonation of the pyridine nitrogen atom of N-(1,1,3,3-tetramethylbutyl)-2-(2pyridylcarbonyl)benzamide, obtained in the open amide form, is accompanied by the closing of the isoindotinone ring; the deprotonation is accompanied by ring opening.Riga Technical University, Riga LV-1048. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 4, pp. 499–504, April, 1994. Original article submitted March 17, 1994.     

Electrohydraulic effect in aqueous-plant heterodisperse systems III. A study of the composition of the solid phase and the aqueous phase

By changing the conditions of the electrohydraulic treatment of aqueous plant heterodisperse systems comparatively high degradation of the lignin component of plant tissue has been achieved. In addition to free monosaccharides, their reduced forms have been detected in the aqueous phase. Institute of the Chemistry of Plant Substances, Academy of Sciences of the Republic of Uzbekistan, Tashkent, fax (3712) 89 14 75. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 795–798, November–December, 1994.     

Electron-impact mass spectra of natural phenylethanoids

The electron-impact mass spectra of a number of phenylpropanoids and iridoid glycosides containing a phenylethanoid fragment in their structure have been studied. This has revealed features of the formation of fragments of 4-hydroxyphenylethyl and 3,4-dihydroxyphenylethyl alcohols and also of fragments of phenylethylamine and indolylethylamine derivatives present in the structures of the compounds investigated.     

Some kinetic features of the hydrolysis of protopectin

Some features of the kinetics of the hydrolysis of apple protopectin have been studied on the basis of an analysis of monosaccharide residues of the pectin substances and determinations of characteristic viscosity. It has been shown that the fine regulation of the physicochemical parameters of the hydrolysis of protopectin leads to the formation of pectin substances with different properties.     

Liquid chromatography and mass spectrometry determination of aromatic amines in hydrolysed urine from workers exposed to thermal degradation products of polyurethane

Chromatographia - An LC-MS method is described for the determination of 4,4′-MDA (4,4′-methylene dianiline) in hydrolysed urine as a biomarker for exposure to 4,4′-MDI...     

Linearization of column responses by correlation chromatography. Separation improvement and reduction of undesired adsorption effects

Summary Experiments and simulations prove that correlation chromatography can greatly reduce the disadvantage of a non-linear response of the chromatographic column. A factor that has been accepted as being an important source of error in correlation or multiplex chromatography, has been shown not to be. Separations affected, improve dramatically when correlation chromatography is used, and a substantial amount of correlation noise only arises when there is a large difference in separation between a conventional chromatogram and a correlogram.A model has been developed for simulating these nonlinearities. It is shown that, especially for correlation chromatography, the simulation results match the practical measurements very well.     

Recent developments in the chemistry of stable doubly bonded germanium compounds

During the last 10 years, several compounds of the type Ge=X (X = C, Ge, N, P, S) have been isolated as monomers. The stabilization of such derivatives, which are generally highly polymerizable, was achieved by using very bulky groups both on the germanium atom and on the heteroelement X. Conjugation (particularly in a few germenes and germaimines) and intramolecular or intermolecular coordination with oxygen or nitrogen, also contributes, in some cases, to the stabilization. The X-ray analyses of such compounds show a significant bond shortening of the double bond (8–10%) relative to the corresponding single bond and a planar or nearly planar germanium. These doubly bonded germanium derivatives are usually thermally stable but must be handled in an inert atmosphere because of their high sensitivity to oxygen and moisture; they are extremely reactive, much more than the corresponding carbon analogues. Nearly quantitative additions on the double bond have been observed with electrophiles and nucleophiles, and various types of cycloadditions also occur. Except in one case, a germylene behavior has not been observed, proving that such compounds retain their structural integrity in solution.