Zur Darstellung von 6-Oxo-2H-pyrano[2,3—c]pyrazolen

By the reaction of 4-dimethylaminomethylene-3-methyl-1-phenylpyrazol-5-one (3) with methylene compounds like malonodinitrile, cyanoacetamide and alkyl cyanoacetate a number of different substituted title compounds may be prepared. The mechanism of this reaction is illucidated by isolation of the intermediate ethenyl compounds7, 8, 11, 14 and16. The reaction therefore is best described as a sequence of addition, elimination and cyclisation with partial hydrolysis.

6. Mitt.:H.-H. Otto undO. Rinus, Arch Pharm. (Weinheim)312, 548 (1979).     

Massenspektroskopie in der Drogenanalyse

The mass spectra of barbituric acid derivatives reflect the high stability of the malonic acid ureide system. Aliphatically substituted derivatives show preferential fragmentation of the substituents while derivatives with aromatic substituents exhibit cleavage of the barbituric acid portion under formation of stable conjugated systems. These observations allow easy identification of this type of compounds. The high sensitivity of mass spectrometers (mikrogram range) together with modern methods for separation (TLC andGLC) render mass spectrometry a potent tool in forensic analysis.     

Cobalt oxide/tetraruthenated cobalt-porphyrin composite for hydrogen peroxide amperometric sensors

A new composite material constituted by mu-{5,10,15,20-tetra(4-pyridyl)porphyrinato cobalt(iii)}-tetrakis-{chloro-bis-(2,2'-bipyridine)ruthenium(ii)} complex (or CoTRP) and cobalt oxide, exhibiting high stability and sensitivity for the quantification of hydrogen peroxide, was obtained by the electrochemical polymerization of the tetraruthenated cobalt porphyrin in alkaline medium. The optimized experimental conditions for the preparation of the modified glassy carbon electrodes and for analysis of H2O2 were carefully determined. Fast sequential analysis (120 determinations h(-1)) in a wide linear dynamic range (5.0 x 10(-7) mol L(-1) to 2.0 x 10(-3) mol L(-1)), with high sensitivity and low detection limit (2.0 x 10(-7) mol L(-1)), was achieved by using these electrodes and the batch injection analysis (BIA) technique. Such characteristics allied to a good stability were explored for the specific determination of hydrogen peroxide in six commercial cosmetics and pharmaceutical product samples, giving results in excellent agreement with those obtained by the spectrophotometric method.     

Weitreichende Anisotropieeffekte bei längerkettigen Amiden

In¹H-NMR spectra of amids with long-chain aliphatic N-substituents one observes—despite of the free mobility of the aliphatic chain—splitting of the signals of the terminal methyl groups which is caused by the hindered rotation of the amide bond.

     

Lokalisierung von Substituenten bei Porphyrinen: Das Massenspektroskopische Fragmentierungsverhalten von Porphyrinogenen

The possibilities and limitations for localization of substituents in porphyrins from the fragmentation patterns of porphyrinogens are discussed.     

Statistical mechanics of the isothermal lane-emden equation

For classical point particles in a box with potential energy H^(N)=N ^–1(1/2) _ij=1 ^N V(x _i,x _j) we investigate the canonical ensemble for largeN. We prove that asN the correlation functions are determined by the global minima of a certain free energy functional. Locally the distribution of particles is given by a superposition of Poisson fields. We study the particular case =[–L, L] andV(x, y)=}- cos(x–y),L}>0, }>0.References     

Subgraphs smaller than the girth

For graphs A, B, let () denote the number of subsets of nodes of A for which the induced subgraph is B. If G and H both have girth > k, and if () = () for every k-node tree T, then for every k-node forest F, () = (). Say the spread of a tree is the number of nodes in a longest path. If G is regular of degree d, on n nodes, with girth > k, and if F is a forest of total spread ≤k, then the value of () depends only on n and d.     

Semiquantitative Autoradiographie mit Hilfe des Ringofens. II

Zusammenfassung Die bereits in einer früheren Mitteilung beschriebene Methode zur halb quantitativen Bestimmung radioaktiver Substanzen mit Hilfe der Chronoautoradiographie wird weiter ausgeführt. Die Genauigkeit und die Empfindlichkeit der Methodik wurden diskutiert und eine Reihe verschiedener Anwendungsbeispiele beschrieben, insbesondere die Anwendung einer aus einem Nuklid hergestellten Standardskala zur Bestimmung anderer Nuklide. Die experimentelle Ermittlung des dazu benötigten Nuklidumrechnungsfaktors wird beschrieben.

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Summary The method described in a previous communication for the semi-quantitative determination of radioactive materials with the aid of chronoautoradiography is further developed. The precision and the sensitivity of the methodology are discussed and a number of instances of application are described, especially the use of a standard scale prepared from an isotope for the determination of other isotopes. The experimental determination of the required isotope conversion factor is described.

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Résumé On a de nouveau étudié la méthode décrite dans une communication précédente pour le dosage semiquantitatif de substances radioactives au moyen de la chronoautoradiographie. On a discuté l'exactitude et la sensibilité de la méthode et décrit une série de plusieurs exemples d'applications, en particulier l'utilisation d'une échelle étalon préparée à partir d'un isotope pour le dosage d'autres isotopes. On décrit la recherche expérimentale du facteur de conversion isotopique nécessaire pour cela.

     

Disperse Ferromagnetika

Zusammenfassung Mischf?llungen eines ferromagnetischen Stoffs (Fe₃O₄ oder Fe) mit unmagnetischen Tr?gerstoffen (Al(OH)₃, Silikagel und SrSO₄) sind um so weniger magnetisierbar, je h?her dispers das Ferromagnetikum darin vorliegt. Durch Alterung bei Zimmertemperatur, schneller noch bei 75⁰, steigt die Magnetisierbarkeit der Niederschl?ge an. Es ist mir eine besondere Freude, auch an dieser Stelle der Unterstützung durch die Vereinigung der F?rderer und Freunde der Universit?t Leipzig bei der Beschaffung des für die Versuche erforderlichen Galvanometers zu gedenken und zugleich auch Herrn Geheimrat Le Blanc für das dabei bewiesene liebenswürdige Interesse herzlich zu danken.