Cu(II) immobilized on Fe3O4–diethylenetriamine: A new magnetically recoverable catalyst for the synthesis of 2,3‐dihydroquinazolin‐4(1H)‐ones and oxidative coupling of thiols

Cu(II) immobilized on Fe₃O₄–diethylenetriamine was designed as a new, inexpensive and efficient heterogeneous catalyst for the synthesis of 2,3‐dihydroquinazolin‐4(1H )‐ones and the oxidative coupling of thiols. The structure of the nanomagnetic catalyst was comprehensively characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, vibrating sample magnetometry, thermogravimetric analysis, X‐ray diffraction and atomic absorption spectroscopy. Simple preparation of the catalyst from commercially available materials, high catalytic activity, simple operation, high yields, use of green solvents, easy magnetic separation and reusability of the catalyst with unaltered activity make our protocol a green and feasible synthetic strategy.     

Enantiopure Ferrocene‐Based Planar‐Chiral Iridacycles: Stereospecific Control of Iridium‐Centred Chirality

Reaction of [IrCp*Cl₂]₂ with ferrocenylimines (Fc=NAr, Ar=Ph, p‐MeOC₆H₄) results in ferrocene C?H activation and the diastereoselective synthesis of half‐sandwich iridacycles of relative configuration S_p*,R_Ir*. Extension to (S)‐2‐ferrocenyl‐4‐(1‐methylethyl)oxazoline gave highly diastereoselective control over the new elements of planar chirality and metal‐based pseudo‐tetrahedral chirality, to give both neutral and cationic half‐sandwich iridacycles of absolute configuration S_c,S_p,R_Ir. Substitution reactions proceed with retention of configuration, with the planar chirality controlling the metal‐centred chirality through an iron–iridium interaction in the coordinatively unsaturated cationic intermediate.     

Die Untersuchung einer Laboratoriumsanlage nach dem Heiß-Kalt-System mit einfachem Durchfluß der Fluide

Es wird ein Heiβ-Kalt-System mit einfachem Durchfluβ der Fluide untersucht. Dabei wird gezeigt, daβ zwischen den Isotopenkonzentrationen des Gases und der Flüssigkeit lineare Beziehungen bestehen. Eine Möglichkeit zur experimentellen Bestimmung der realen Werte der Parameter der Kolonne wird angegeben.     

Interaction Products of 12·5 Deuterons with Molybdenum and their Isolation Possibilities from Worn-out Cyclotron Parts

Using chemical separations and radiometric measurements medium-half-life irradiation products of molybdenum with 12.5 MeV deuterons were determined (⁹⁰Nb, ⁹²Nb, ^95mNb, ⁹⁵Nb, ⁹⁶Nb, ⁹⁹Mo, ^95mTc, ⁹⁶Tc, ^99mTc) as well as thick target yields for some of them: ⁹²Nb (0.22 μCi/μAh), ⁹⁵Nb(0.05 μCi/μAh), ⁹⁹Mo (64 μCi/μAh), ^95mTc(0.76 μCi/μAh), ⁹⁶Tc((62.5 μCi/μAh). Moreover isolation possibiities of radioactive preparations from removed worn-cut molybdenum parts of the U-120 cycletron are discussed.     

Doubly N‐Confused [36]Octaphyrin(1.1.1.1.1.1.1.1): Isomerization,Bis‐Metal Coordination,and Topological Chirality

A novel [36]octaphyrin analogue embedding two N‐confused pyrrole units demonstrated unique prototropy‐coupled isomerization between the Figure‐of‐eight and dumbbell conformers. Upon bis‐metal coordination, fixation of fully π‐conjugated Figure‐of‐eight structures was achieved as referred from the X‐ray crystal structure. Chirogenesis of the helical enantiomers was proved by intense circular dichroism (CD) response in the near infrared (NIR) region.     

Enantiomeric separation of 2‐arylpropionic acid nonsteroidal anti‐inflammatory drugs by HPLC with hydroxypropyl‐β‐cyclodextrin as chiral mobile phase additive

The enantio‐separations of eight 2‐arylpropionic acid nonsteroidal anti‐inflammatory drugs (2‐APA NSAIDs) were established using reversed‐phase high‐performance liquid chromatography with hydroxypropyl‐β‐cyclodextrin (HP‐β‐CD) as chiral mobile phase additive for studying the stereoselective skin permeation of suprofen, ketoprofen, naproxen, indoprofen, fenoprofen, furbiprofen, ibuprofen and carprofen. The effects of the mobile phase composition, concentration of HP‐β‐CD and column temperature on retention and enantioselective separation were investigated. With 2‐APA NSAIDs as acidic analytes, the retention times and resolutions of the enantiomers were strongly related to the pH of the mobile phase. In addition, both the concentration of HP‐β‐CD and temperature had a great effect on retention time, but only a slight or almost no effect on resolutions of the analytes. Enantioseparations were achieved on a Shimpack CLC‐ODS (150 × 4.6 mm i.d., 5 μm) column. The mobile phase was a mixture of methanol and phosphate buffer (pH 4.0–5.5, 20 mM) containing 25 mM HP‐β‐CD. This method was flexible, simple and economically advantageous over the use of chiral stationary phase, and was successfully applied to the enantioselective determination of the racemic 2‐APA NSAIDs in an enantioselective skin permeation study. Copyright © 2009 John Wiley & Sons, Ltd.     

Fields,particles and universality in two dimensions

We discuss the use of field theory for the exact determination of universal properties in two-dimensional statistical mechanics. After a compact derivation of critical exponents of main universality classes, we turn to the off-critical case, considering systems both on the whole plane and in presence of boundaries. The topics we discuss include magnetism, percolation, phase separation, interfaces, wetting.     

Explicit–implicit mapping approach to nonlinear blind separation of sparse nonnegative dependent sources from a single mixture: pure component extraction from nonlinear mixture mass spectra

The nonlinear, nonnegative single‐mixture blind source separation problem consists of decomposing observed nonlinearly mixed multicomponent signal into nonnegative dependent component (source) signals. The problem is difficult and is a special case of the underdetermined blind source separation problem. However, it is practically relevant for the contemporary metabolic profiling of biological samples when only one sample is available for acquiring mass spectra; afterwards, the pure components are extracted. Herein, we present a method for the blind separation of nonnegative dependent sources from a single, nonlinear mixture. First, an explicit feature map is used to map a single mixture into a pseudo multi‐mixture. Second, an empirical kernel map is used for implicit mapping of a pseudo multi‐mixture into a high‐dimensional reproducible kernel Hilbert space. Under sparse probabilistic conditions that were previously imposed on sources, the single‐mixture nonlinear problem is converted into an equivalent linear, multiple‐mixture problem that consists of the original sources and their higher‐order monomials. These monomials are suppressed by robust principal component analysis and hard, soft, and trimmed thresholding. Sparseness‐constrained nonnegative matrix factorizations in reproducible kernel Hilbert space yield sets of separated components. Afterwards, separated components are annotated with the pure components from the library using the maximal correlation criterion. The proposed method is depicted with a numerical example that is related to the extraction of eight dependent components from one nonlinear mixture. The method is further demonstrated on three nonlinear chemical reactions of peptide synthesis in which 25, 19, and 28 dependent analytes are extracted from one nonlinear mixture mass spectra. The goal application of the proposed method is, in combination with other separation techniques, mass spectrometry‐based non‐targeted metabolic profiling, such as biomarker identification studies. Copyright © 2015 John Wiley & Sons, Ltd.