Ein neues makrobicyclisches Wirtmolekül-Synthese und ANS-Komplexierung

The synthesis of the new host molecule1b is described. Its complexation properties towards 1,8-ANS as a guest are reported. Compared to the monomacrocyclic host molecules2c and2e, the complex stabilities of1b with ANS as a guest are particularly higher, suggesting that the macrobicyclic host forms a better fitting niche to allow the nestling of guest molecules in solution.

     

Cyclodextrine und synthetische Wirthohlräume — Vergleich der Komplexierungseigenschaften

It is shown that the synthetic host compounds described in this study possess higher complexation constants versus 1,8-ANS than -or -cyclodextrin. The attachment of side chains to -cyclodextrin increases the complex formation, whereas the value of -cyclodextrin is not reached. The quaternary ammonium nitrogens of the synthetic hosts may be replaced by amide groups without diminution of the association constants. Bicyclic compounds in general bind more strongly than monocyclic hosts due to tighter inclusion and increased hydrophobic interaction. The influence of side chains attached to synthetic host compounds on the complexation constants is difficult to predict.

     

Gasanalyse

Ohne Zusammenfassung     

Ein neues Verfahren zur quantitativen Bestimmung der Weins?ure im Wein

Ohne Zusammenfassung     

ZnO homoepitaxy on the O polar face of hydrothermal and melt-grown substrates by pulsed laser deposition

2 cm diameter hydrothermal ZnO crystals were grown and then made into substrates using both mechanical and chemical-mechanical polishing (CMP). CMP polishing showed superior results with an (0002) Ω scan full width half maximum (FWHM) of 67 arcsec and an root mean square (RMS) roughness of 2 Å. In comparison, commercial melt-grown substrates exhibited broader X-ray diffraction (XRD) linewidths with evidence of sub-surface crystal damage due to polishing, including a downward shift of c-lattice parameter. Secondary ion mass spectroscopy revealed strong Li, Fe, Co, Al and Si contamination in the hydrothermal crystals as opposed to the melt-grown substrates, for which glow discharge mass spectroscopy studies had reported high levels of Pb, Fe, Cd and Si. Low temperature photoluminescence (PL) studies indicated that the hydrothermal crystal had high defect and/or impurity concentrations compared with the melt-grown substrate. The dominant bound exciton for the melt-grown substrate was indexed to Al. ZnO films were grown using pulsed laser deposition. The melt-grown substrates gave superior results with XRD (0002) Ω and 2θ/Ω WHM of 124 and 34 arcsec, respectively. Atomic force microscope measurements indicated a low RMS roughness (1.9 nm) as confirmed by fringes in the XRD 2θ/Ω scan. It was suggested that the improvement in XRD response relative to the substrate might be due to “healing” of sub-surface polishing damage due to the elevated T_s used for the growth. Indeed the c-lattice parameter for the homoepitaxial layer on the melt-grown substrate had become that which would be expected for strain-free ZnO. Furthermore, the stability of the PL peak positions relative to bulk ZnO, confirmed that the films appear practically strain free.     

Bücherbesprechungen

Ohne Zusammenfassung     

A study on UV laser drilling of PEEK reinforced with carbon fibers

This paper deals with the application of Nd-YAG laser emitting at 355 nm to the drilling process of Carbon Fiber Reinforced Polyetheretherkethone (PEEK-CF) laminates. The combination of a modern UV-laser source with a scanning technology enabling speeds up to 4 m/s, suppresses heat affected zones (HAZ) and consequently detachment of fibers from the polymer matrix. A removal technique based on the ablation of superimposed layers of composite material is proposed and analyzed in detail as a function of energy density delivered to the surface, hatch strategy and thickness of the laminate to be drilled. The hatching technique discussed in the paper is compared with conventional laser trepanning and percussion drilling through holes for the realization of 2 mm and 0.1 mm diameter, respectively. In both the cases benefits were noticed in terms of extension of HAZ and quality of the cut edges.     

Improvements to the compressed-sample (CS) technique for MALDI-TOF mass spectrometry

A recently developed solvent-free compressed-sample technique for matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS) analysis allows the reproducible analysis of synthetic polymers and peptides up to 3,500 Da. In this work, we present an improvement in resolution, an increase in intensity and a decrease of the variation coefficient, as illustrated by the analysis of PEG 2000 and MALDI imaging experiments. These advantages were achieved by homogenization of the electrical field, which was disturbed by the drills in the original MALDI target. In order to homogenize the electrical field, a new target with smaller drills was developed, metal powder was added to the matrix/analyte mixture and a round laser raster was used. Furthermore, a ball mill was implemented for the sample preparation to replace the extremely user-dependent grinding in a mortar. The new conditions were successfully applied to the quantification of several peptides of higher molecular weight and gave higher precision than had previously been achieved with the compressed-sample technique.     

Structure-Based Evolution of Subtype-Selective Neurotensin Receptor Ligands

Subtype-selective agonists of the neurotensin receptor NTS2 represent a promising option for the treatment of neuropathic pain, as NTS2 is involved in the mediation of μ-opioid-independent anti-nociceptive effects. Based on the crystal structure of the subtype NTS1 and previous structure–activity relationships (SARs) indicating a potential role for the sub-pocket around Tyr11 of NT(8–13) in subtype-specific ligand recognition, we have developed new NTS2-selective ligands. Starting from NT(8–13), we replaced the tyrosine unit by β²-amino acids (type 1), by heterocyclic tyrosine bioisosteres (type 2) and peptoid analogues (type 3). We were able to evolve an asymmetric synthesis of a 5-substituted azaindolylalanine and its application as a bioisostere of tyrosine capable of enhancing NTS2 selectivity. The S-configured test compound 2 a, [(S)-3-(pyrazolo[1,5-a]pyridine-5-yl)-propionyl¹¹]NT(8–13), exhibits substantial NTS2 affinity (4.8 nm) and has a nearly 30-fold NTS2 selectivity over NTS1. The (R)-epimer 2 b showed lower NTS2 affinity but more than 600-fold selectivity over NTS1.