Regioselective synthesis of pyrrolin-3-ones and 2,3,4,5-tetrahydro[1,3]-oxazines from N-vinylic amidines

Achiral and optically active N-vinylic amidines are obtained by simple addition of amidines to acetylenic esters. Thermal intramolecular cyclization of these substrates containing a carboxylate group in position 3 gives pyrrolin-3-ones. The enaminone character of these compounds towards propargyl bromide, diethyl azodicarboxylate, diethyl acetylenedicarboxylate, ethyl propiolate and phenyl isocyanate is studied and functionalized pyrrolin-3-one derivatives are obtained. The reaction of the pyrrolinones prepared with diethyl ketomalonate leads to new 1,3-oxazine derivatives.     

Critical distance for secondary ion formation: Experimental SIMS measurements

We have performed direct experimental measurements of the critical distance for the secondary ion formation process. To this end, we compared the experimentally measured energy distribution of secondary Si⁻ ions with the theoretical energy distribution (Sigmund-Thompson relation) of secondary Si atoms. Our model states that the maxima positions of these two energy distributions differ by the Coulomb interaction potential between the outgoing ion (Si⁻ in our case) and a charge with the opposite polarity formed at the surface after electron transition between the outgoing Si atom and the surface. Quite a reasonable value was obtained for the critical distance, but with a large scatter in experimental data. The conclusion has been made that the experimental technique should be improved to get more precise values of the critical distance, which is of high importance for practical purposes.     

Lyapunov-type Inequalities for Differential Equations

Let us consider the linear boundary value problem

Two new conformationally restricted 4,5‐dihydroxynorvaline analogues with a norbornane skeleton

The structures of two conformationally restricted 4,5‐di­hydroxy­norvaline analogues with a norbornane skeleton, namely methyl (1S,2S,3R,4R)‐2‐benz­amido‐3‐(1,2‐di­hydroxy­ethyl)­bi­cyclo[2.2.1]­heptane‐2‐carboxyl­ate, C₁₈H₂₃NO₅, and methyl (1R,2S,3R,4S)‐2‐benz­amido‐3‐(1,2‐di­hydroxy­ethyl)­bi­cyclo[2.2.1]­heptane‐2‐carboxyl­ate, C₁₈H₂₃NO₅, exhibit a conformation in the helical region of the ?,ψ map but their handedness is opposite. In both cases, the torsion angles (χ^1,1) giving the relative orientation of the 1,2‐di­hydroxy­ethyl group of the amino acid side chain and the benz­amide group of the peptide chain indicate that these groups adopt a nearly eclipsed conformation. Both compounds show a complex hydrogen‐bonding pattern.     

Boundedness of extremal solutions in dimension 4

In this paper we establish the boundedness of the extremal solution u^∗$u^{\ast }$ in dimension N=4$N=4$ of the semilinear elliptic equation −Δu=λf(u)$-\Delta u=\lambda f\left(u\right)$, in a general smooth bounded domain Ω⊂R^N$\Omega \subset {\mathbb{R}}^N$, with Dirichlet data u_|∂Ω=0$u{|}_{\partial \Omega }=0$, where f$f$ is a C¹$C^1$ positive, nondecreasing and convex function in [0,∞)$[0,\infty )$ such that f(s)/s→∞$f\left(s\right)/s\to \infty$ as s→∞$s\to \infty$.     

On the effect of flat energy directors thickness on heat generation during ultrasonic welding of thermoplastic composites

This paper presents a detailed experimental assessment of the effect of the thickness of flat energy directors (ED) on heat generation at the interface during ultrasonic welding. Power and displacement data showed clear differences caused by the change of thickness, related to heat concentration at the weld line during the process. The extent of the heat-affected zone was assessed by welding specimens without consolidation at different stages of the process. It was confirmed through optical microscopy that heat is generated at the interface and transferred to the bulk adherends earlier in the process for thinner ED. The analysis of their fracture surface under optimum welding conditions revealed signs of matrix degradation, leading to less consistent quality, likely due to faster heat generation rate in both the ED and the substrates, and incidentally, higher temperatures surrounding the energy director.     

Modification and intercalation of layered zirconium phosphates: a solid‐state NMR monitoring

Several layered zirconium phosphates treated with Zr(IV) ions, modified by monomethoxy‐polyethyleneglycol‐monophosphate and intercalated with doxorubicin hydrochloride have been studied by solid‐state MAS NMR techniques. The organic components of the phosphates have been characterized by the ¹³C{¹H} CP MAS NMR spectra compared with those of initial compounds. The multinuclear NMR monitoring has provided to establish structure and covalent attachment of organic/inorganic moieties to the surface and interlayer spaces of the phosphates. The MAS NMR experiments including kinetics of proton‐phosphorus cross polarization have resulted in an unusual structure of zirconium phosphate 6 combining decoration of the phosphate surface by polymer units and their partial intercalation into the interlayer space. Copyright © 2016 John Wiley & Sons, Ltd.     

Probability of ionization of sputtered particles as a function of their energy: Part I: Negative Si ions

In this study we have investigated how the probability of ionization of sputtered Si atoms to form negative ions depends on the energy of the atoms. We have determined the ionization probability from experimental SIMS energy distributions using a special experimental technique, which included de-convolution of the energy distribution with an instrumental transmission function, found by separate measurements.We found that the ionization probability increases as a power law ∼E^0.677 for particles sputtered with energies of 0-10 eV, then becomes a constant value (within the limits of experimental error) for particles sputtered with energies of 30-100 eV. The energy distributions of Si⁻ ions, measured under argon and cesium ion sputtering, confirmed this radical difference between the yields from low and high-energy ions.To explain these results we have considered ionization mechanisms that are different for the low energy atoms (<10 eV) and for the atoms emitted with higher energy (>30 eV).     

A representation of recursively enumerable sets through Horn formulas in higher recursion theory

We prove the existence of graphs with empty intersection of their longest paths or cycles as subgraphs of lattices on the torus and the Möbius strip.     

New layered double hydroxides containing intercalated manganese oxide species: synthesis and characterization

Manganese oxide species (MnO(x)) have been intercalated within the gallery spaces of Mg-Al layered double hydroxides (LDHs). Synthesis of these materials was achieved by ion-exchange of the LDH-nitrate precursor with permanganate anion followed by reduction with organic reagents, such as glucose, ethanol, and ascorbic acid. Elemental analysis, X-ray diffraction, FT-IR spectroscopy, Raman spectroscopy, HR-TEM, and N(2) sorption analyses have been used to characterize these materials. TEM micrographs of LDH-MnO(x) materials revealed platelike morphology, characteristic of hydrotalcite-like compounds. Chemical analysis results showed that permanganate anions exchanged with nitrate anions. FT-IR and Raman spectroscopy confirmed the reduction of the permanganate anions after treatment with the organic reagents. The XRD diffraction patterns of LDH-MnO(x) revealed that the layer structure is maintained after all synthetic steps. The observed basal spacings of intercalates varied depending on the reducing agent; the largest expansion was 9.93A, corresponding to the use of ascorbic acid. The specific surface areas were also affected according to the organic reagent used, indicating that the structural modifications in the interlayer domain observed by X-ray diffraction also influence the microtextural properties.