A General Catalyst Based on Cobalt Core–Shell Nanoparticles for the Hydrogenation of N-Heteroarenes Including Pyridines

Herein, we report the synthesis of specific silica-supported Co/Co₃O₄ core–shell based nanoparticles prepared by template synthesis of cobalt-pyromellitic acid on silica and subsequent pyrolysis. The optimal catalyst material allows for general and selective hydrogenation of pyridines, quinolines, and other heteroarenes including acridine, phenanthroline, naphthyridine, quinoxaline, imidazo[1,2-a]pyridine, and indole under comparably mild reaction conditions. In addition, recycling of these Co nanoparticles and their ability for dehydrogenation catalysis are showcased.     

Enantioselective hydrogenation of diaryl-substituted α,β-unsaturated nitriles

α,β-Unsaturated nitriles can be hydrogenated with enantioselectivities up to 88% ee using chiral ruthenium-diphenylphosphino bisaryl and bisheteroaryl complexes such as ruthenium(II)-BINAP and ruthenium(II)-BINP. Mechanistic investigations indicate that conversion is accelerated by electron-rich ligands and that an additional coordinative group needs be present in order to promote conversion. The chiral products are useful building blocks for the synthesis of histamine H₂ agonists of the arpromidine type.     

Determination of residual solvents in a transdermal system by means of headspace gas chromatography

Summary Pharmaceutical products have to be tested for impurities including residual solvents. This is also required in production control. The simplest solution to this problem is headspace gas chromatography. This paper describes the determination of residual volatile hydrocarbons in the transdermal system DEPONIT by only one headspace measurement. Accuracy is ensured by the multiple headspace extraction technique.

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Bestimmung von Restlösungsmittelgehalten in einem transdermalen System durch Headspace-Gas-Chromatographie

Zusammenfassung Pharmazeutische Produkte müssen auf Verunreinigungen geprüft werden, auch auf Restlösungsmittelgehalte. Ein zusätzlicher Grund ist die fortlaufende Kontrolle der Herstellung. Die einfachste Möglichkeit für dieses Problem ist die Bestimmung durch Headspace-Gas-Chromatographie. Dieser Artikel beschreibt die Bestimmung von noch vorhandenen flüchtigen Kohlenwasserstoffen in dem transdermalen System DEPONIT durch nur eine Headspace-Messung. Die Richtigkeit ist durch die Anwendung der Mehrfach-Gasextraktionstechnik sichergestellt.

     

Discrete approximation of integral operators

A method to approximate the eigenvalues of linear operators depending on an unknown distribution is introduced and applied to weighted sums of squared normally distributed random variables. This area of application includes the approximation of the asymptotic null distribution of certain degenerated U- and V-statistics.

     

A high sensitivity titration calorimeter using pyroelectric sensor

A new sensitive isothermal titration microcalorimeter using polyvinylidene difluoride (PVDF) as detector has been developed. Heat pulses of less than 0.4 μJ can be detected and the baseline noise level (p-p) is 40 nW. The calorimeter is constructed with one reaction cell (0.7 ml) insulated by several radiation shields inside a vacuum chamber. The performance of the instrument was examined by measuring the heat of protonation of Tris with HCl. The enthalpy of reaction was found to be ?49±1 kJ·mol^?1, in good agreement with the reported value of ?47.5 kJ·mol^?1.     

A Simpler Proof of the Excluded Minor Theorem for Higher Surfaces

We give a simple proof of the fact (which follows from the Robertson–Seymour theory) that a graph which is minimal of genusgcannot contain a subdivision of a large grid. Combining this with the tree-width theorem and the quasi-wellordering of graphs of bounded tree-width in the Robertson–Seymour theory, we obtain a simpler proof of the generalized Kuratowski theorem for each fixed surface. The proof requires no previous knowledge of graph embeddings.