5,6-Dimethoxy- und [4,5,6-Trimethoxy-benzo[b]-thienyl-(3)]-acylamine

Zusammenfassung Umsetzung von 5,6-Dimethoxy- und [4,5,6-Trimethoxy-benzo[b]thienyl-(3)]-essigsäure mit PCl₅ lieferte die methoxysubstituierten [Benzo[b]thienyl-(3)]-essigsäurechloride, die mit sekundären Aminen zu den entsprechenden Amiden reagierten.Die homologen Verbindungen mit einer C₃-Brücke wurden durchArndt-Eistert-Reaktion des Diazomethylketons in Gegenwart der entsprechenden sekundären Amine erhalten.

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Reaction of 5.6-dimethoxy- and [4.5.6-trimethoxybenzo[b]-thienyl-(3)]-acetic acid with PCl₅ gave the methoxy-substituted [benzo[b]thienyl-(3)]-acetic acid chlorides, which reacted with secondary amines to the corresponding amides.The homologous compounds with a C₃-bridge were synthesized viaArndt-Eistert reaction of the diazomethyl ketone in presence of the corresponding secondary amines.

     

Synthesis and structural characterization of acetatobis(triphenylphosphine)dicarbonylmanganese(I), (CH3CO2)Mn(CO)2[P(C6H5)3]2: An organometallic complex containing a chelating acetate ligand

The accidental but intriguing synthesis of acetatobis(triphenylphosphine)dicarbonylmanganese(I), (CH₃CO₂)Mn(CO)₂[P(C₆H₅)₃]₂, has been accomplished by the reaction of NaMn(CO)₅ with (CH₃)₃SiCl followed by the addition of triphenylphosphine and acetic acid. A three-dimensional single-crystal X-ray diffraction analysis has shown an octahedral-like molecule containing a symmetrically oxygen-chelating acetate group, the first such group to be reported in a metal carbonyl complex. The two triphenylphosphine ligands occupy mutually trans positions with the two carbonyl ligands possessing the remaining cis sites in the octahedral complex. The compound crystallizes with four molecules in a monoclinic unit cell of space group symmetry $\text{P}\text{2}{}_1\text{c}$ and of dimensions a = 17.744(2) Å, b = 9.692(1) Å, c = 20.004(2) Å, and β = 106.195(4)°. The relatively long MnO(acetate) bond lengths [2.066(6) and 2.069(7) Å] and the relatively short MnCO bond lengths [1.701(12) and 1.760(13) Å] and the relatively short MnP(C₆H₅)₃ bond lengths [2.260(3) and 2.275(3) Å], compared to the corresponding MnCO and MnP(C₆H₅)₃ bond lengths in other manganese carbonyl triphenylphosphine complexes, are rationalized on the basis that the acetate ligand in this molecule functions primarily as a σ-donor.     

Pfropfcopolymerisation von Cellulose mit zwei Vinylmonomeren

Zusammenfassung Die vorliegende Arbeit stellt eine Beschreibung von Experimenten dar, die die Erhöhung der Pfropfbereitschaft von trägen Komponenten durch Beimischung von aktiveren zum Ziele hatten.Das Trägermolekül war in allen Fällen Cellulose in Form von hochgradig gereinigtem Zellstoff. Durch die Verwendung von Mischsystemen aus Styrol und Methylmethacrylat gelang es, das trägere Styrol in bedeutend größerer Menge auf die Cellulose aufzupfropfen, als es bei Abwesenheit des aktiven Methylmethacrylats der Fall war.

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Grafting Polymerization of Cellulose with Two Vinyl Monomers

This paper describes experiments to increase the grafting of cellulose with components of poor reactivity by mixing them with highly reactive ones. A highly purified wood pulp was used as backbone. Using combinations of styrene and methyl methacrylate it was possible to graft considerably higher amounts of the poorly reacting styrene than in the absence of the highly reactive methyl methacrylate.

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Nach einem Vortrag, den der erstgenannte der Autoren im Rahmen der Arbeitstagung des Vereins Österreichischer Chemiker am 27. September 1968 in Wien gehalten hat.     

Intradiffusion coefficients in perchloric acid solutions: Water at 5°C; water and perchlorate ion at 25°C

Intradiffusion coefficients for tritiated water (³HHO) and perchlorate ion (³⁶ClO ₄ ^- ) were measured in perchloric acid solutions. At 5°C the diffusion coefficient measured for the tritiated species increases to a maximum near 1.3 mol-dm^–3. The data at 25°C have been used to calculate distinct diffusion coefficients, D _ij ^d . As a precursor for those calculations, new estimates were made of the Onsager phenomenological coefficients, l _ij . The l _ij and D _ij ^d are similar to the respective coefficients in hydrochloric acid solutions.     

Theory for migration of ions in capillary electrochromatography

The fundamental migration theories for chromatography and electrophoresis are both based on a solution of the mass balance equation. The corresponding analysis for an electrochromatographic system has previously been published and is analysed in more detail in this paper. It is shown that the resulting equation, Eq. (8) in this paper, is in agreement with both electrophoretic and chromatographic theories and that when these migration modes are mixed a complicated migration behaviour emerge. These complications arise, if the comparison is done with electrophoretic theory, because the presence of the stationary phase creates a number of new restrictions on the system (electroneutrality on the stationary phase and simultaneous equilibrium for all components between the eluent and stationary phase). From a mathematical point of view, these restrictions make it difficult for the system to satisfy the coherence condition and this in turn may lead to an anomalous behaviour. To minimise the possibility for a complicated behaviour it is advisable to avoid too much mixing of the two migration mechanisms and/or to match the mobilities of the ionic components in the eluent phase with the mobility of the analyte ion.