Palladium-catalysed 5-endo-trig allylic (hetero)arylation

A palladium-catalysed intramolecular allylic (hetero)arylation strategy for the synthesis of fused cyclopentenes incorporated with all-carbon quaternary and spiro centres is described. The method is straightforward, shows broad scope, proceeds in synthetically useful yields, and provides a rare means to construct complex cyclopentanoids. The reaction is believed to involve a kinetically unfavourable 5-endo-trig carbocyclisation of the tethered (π-allyl)palladium system. Further, this method was successfully applied as the key step in the total synthesis of diterpene natural products taiwaniaquinone H and dichroanone.

A palladium-catalysed intramolecular allylic (hetero)arylation strategy for the synthesis of fused cyclopentenes incorporated with all-carbon quaternary and spiro centres is described.     

Dual-label autoradiographic analysis of human skin fibroblast and myoblast proteins by two-dimensional polyacrylamide gel electrophoresis using immobilised pH gradients in the first dimension

Horizontal two-dimensional polyacrylamide gel electrophoresis with immobilised pH gradients in the first dimension has been applied to the analysis of human skin fibroblast and muscle myoblast total cell proteins. Excellent two-dimensional separations of skin fibroblast proteins were obtained using pH 4-10 immobilised pH gradient gels with a long interelectrode distance (16 cm), but resolution was degraded, particularly of the more acidic proteins, by the use of shorter (10 cm) gels. Improved resolution of acidic and basic proteins was obtained using separate pH 4-7 and pH 7-10 immobilised pH gradient gels respectively in the first dimension. Two-dimensional protein maps of skin fibroblast proteins were visualised both by silver staining and by autoradiography of samples labelled synthetically with [35S]methionine. Horizontal two-dimensional electrophoresis, using pH 4-7 and pH 7-10 immobilised pH gradient gels in the first dimension, was applied to the analysis of protein samples from skin fibroblasts and muscle myoblasts dual-labelled synthetically with [35S]methionine and [75Se]selenomethionine in an attempt to identify sets of proteins specific to each cell type. In addition, two-dimensional maps or protein samples derived from normal individuals and patients with Duchenne muscular dystrophy were compared to search for protein changes associated with the disease state. Although sets of qualitative protein spot differences were observed by visual inspection of the two-dimensional gels, more rigorous qualitative and quantitative analysis of the patterns using a computerised analysis system will be required to obtain the maximum amount of information from these data.     

HPTLC Method for Quantification of Apigenin in the Dried Root Powder of Gmelina arborea Linn.

JPC – Journal of Planar Chromatography – Modern TLC - A sensitive high-performance thin-layer chromatographic method has been established for quantification of apigenin in dried root...     

Synthesis and Biological Activity of 3-[4H-(1,2,4)-Triazolyl]-2,6-diaryl-1,3,5-oxadiazine-4-thione

4-Amino-1,2,4-triazole (1) undergoes facile condensation with aromatic aldehydes to afford the corresponding 4-(arylidene-amino)-4H-[1,2,4]-triazole (2a–h) in good yield. Rearrangement of compounds (2a–h) with benzoyl isothiocyanate/4-chloro-benzoyl isothiocyanate/2,4-dichloro-benzoyl isothiocyanate yields corresponding 1,3,5-oxadiazine derivatives (3). Structural elucidation of these compounds was based on elementary analysis and spectral data studies. The newly synthesized compounds were evaluated for their antibacterial activities.     

Synthesis and thermal studies of bisphenol-A based bismaleimide

The compound 2,2-bis[4-(4-maleimidophenoxy phenyl)]propane was prepared by the imidization of bisamic acid of 2,2-bis(4-aminophenoxy phenyl)propane. Various nanoclays were blended with this bismaleimide and thermally cured. The structural characterization of the synthesized materials and the thermal properties of the bismaleimide and their blends were investigated through FTIR, ¹H and ¹³C NMR, differential scanning calorimetry and thermo gravimetric analysis. Among the various clays investigated, Cloisite 15A shows strong influence on the cure exotherm of bismaleimide. Introduction of clay mineral into bismaleimide shifts the onset of curing exotherm to higher temperature and is nearly 40 °C. The thermal stability of the clay loaded cured bismaleimide increases and the presence of clay particles in the cured bismaleimide matrix enhances the char formation.     

Use of a crown ether-heteropoly acid precipitate as a potassium ion-selective membrane electrode

Summary A Potassium ion-selective electrode based on dibenzo-18-crown-6-tungstophosphoric acid precipitate membrane is prepared and conditions for the best functioning have been investigated. The working concentration and pH-range of the electrode is 2.0×10^–2 to 1.3×10^–6 mol/l and 2.9–6.5, respectively. The selectivity coefficient values for a large number of cations are quite low except for caesium and ammonium ions. The electrode can tolerate non-aqueous content upto 20%.

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Kaliumion-sensitive Membranelektrode auf Basis von Kronenether-Heteropolysäure

     

Isotropic distributions of test matrices

In 1946, von Neumann and his collaborators used a special distribution of random matrices as a model for estimatinga priori the machine precision needed to solve large linear systems. The present paper identifiesisotropy as a group-theoretic property of this distribution, shows that its matrices are almost never ill-conditioned, and explains how to use other isotropically distributed random matrices for testing the accuracy of numerical methods for solving linear systems and associated error diagnostics.

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Zusammenfassung Die zur Lösung linearer Gleichungssysteme benötigte Genauigkeit wurde schon 1946 durch von Neumann und seine Mitarbeiter mittels speziell verteilter Zufallsmatrizen geschätzt. In der vorliegenden Arbeit erscheint dieIsotropie als gruppentheoretische Eigenschaft dieser Verteilung. Ferner wird gezeigt, dass die Zufallsmatrizen fast nie schlecht konditioniert sind. Schliesslich diskutieren die Autoren die Verwendung anderer isotrop verteilter Zufallsmatrizen zur Prüfung von Genauigkeit und a-priori-Fehlerschranken bei Algorithmen zur Lösung linearer Gleichungssysteme.

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Dedicated to Eduard Stiefel

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The main results of this paper were reported in [3], and communicated in 1976 to those working on the LINPACK project.