Cleavage of the C---Se bond of cyclic selenoacetals derived from 4-t-butyl cyclohexanone with butyllithiums and tin and silyl hydrides

Selenoacetals derived from 1,3-propanediselenol and 1,2-ethanediselenol are much less prone to be cleaved by butyllithiums than their open chain analogues. The stereochemistry of the products resulting from these reactions as well as from the cleavage of the C---Se bond under radical conditions is disclosed.     

The synthesis of 3-bromo-2,4,5-trifluorobenzoic acid and its conversion to 8-bromoquinolonecarboxylic acids

A series of 8-bromo-4-oxo-3-quinolinecarboxylic acids was prepared via the borate ester, 8 . The key intermediate in the synthesis of the final products 10a-10d was 3-bromo-2,4,5-trifluorobenzoic acid ( 3 ), conveniently prepared in two steps from the known oxazoline, 1 . The preparation of 10a-10d is a significant improvement of the literature procedure currently available for the synthesis of these compounds.     

Elaboration of ZnO Thin Films with Preferential Orientation by a Soft Chemistry Route

Microcrystalline ZnO films presenting well-defined and tunable orientation were obtained by spin coating of alcoholic sols by two different approaches, based on controlled hydrolysis-condensation of Zn-ethanolamine complexes. As-deposited films are formed by amorphous zinc oxide-acetate submicronic particles, which are transformed into oriented ZnO after thermal treatment. The orientation of ZnO depends on the synthesis method, and the solvent. While in ethanol and [Zn] = 0.05 mol·L^–1, films consist of rectangular platelets oriented with the (100) planes parallel to the substrate (a//n), the orientation of the particles changes to (c//n) for systems in 2-methoxyethanol (2-ME) and [Zn] = 0.75 mol·L^–1. A study of chemical factors that influence the orientation (precursor, solvent, MEA/Zn ratio, concentration, coating parameters, heat treatment) is presented.     

Mikrochemie

Ohne Zusammenfassung     

Highly ordered metal oxide nanopatterns prepared by template-assisted chemical solution deposition

TiO₂, Al₂O₃, and ZrO₂ patterns composed of ordered nano motifs of various morphologies (i.e. perforations (craters), rings, canyons, wires, dots, or channels) with typical lateral dimensions of less than 40 nm and thickness below 15 nm are presented. Simple chemical solution deposition (CSD) of molecular inorganic precursors and commercial block copolymers was used to create patterns on several substrate surfaces (bare, hydrophobized or gold covered silicon wafers and ITO). Self-assembly during evaporation and subsequent stabilization at 500 °C leads to the various nanostructures. Compared to other techniques for surface nano patterning, the present method has the advantage of being cheap, reproducible and easy to scale up and does not require specialized equipment. The type, dimension, and organization of these motifs were assessed by AFM, FE-SEM, spectroscopic ellipsometry, and GI-SAXS and are shown to depend on the conditions of preparation. Usage as model surfaces for modelling of wetting properties and as nanoelectrode arrays were investigated.     

Functionalization of carbon nanofibers (CNFs) through atom transfer radical polymerization for the preparation of poly(tert‐butyl acrylate)/CNF materials: Spectroscopic,thermal, morphological,and physical characterizations

Vapor‐grown carbon nanofibers (CNFs) were oxidized and functionalized for atom transfer radical polymerization (ATRP) of tert‐butyl acrylate (t‐BA) from the surface of the CNFs. The materials were characterized by solubility tests, Fourier‐transform infrared (FTIR) spectroscopy, Raman spectroscopy, thermogravimetric analysis (TGA), X‐ray diffraction (XRD), and scanning electron microscopy. The FTIR and electron microscopy results suggest that ATRP process was successfully used to graft poly(tert‐butyl acrylate) (poly(t‐BA)) chains from the surface of the fibers. Raman results strongly indicate the partial degradation of the graphitic layer of CNFs because of the chemical treatments. TGA results suggest that the presence of poly(t‐BA) leads to a decrease of the initial degradation temperature of the fibers. XRD and electron microscopy results indicate that the microstructure of fibers was not destroyed because of the oxidation and functionalization processes. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 3326–3335, 2008     

Determination de Susceptibilites Paramagnetiques par les Methodes de RMN

Magnetic susceptibilities play a very important part in NMR spectra, but their values are not always known; here, the authors give a method for the measurement of paramagnetic susceptibilities and suggest an explanation about linear dependence of magnetic susceptibility vs. observed shift.     

A simple method for the spectrophotometric determination of chloride by solvent extraction as chromyl chloride

Summary A simple and direct method for the spectrophotometric determination of chloride, based on the formation of chromyl chloride and its extraction into carbon tetrachloride has been developed. The absorption spectrum of the organic extract shows two bands at 300 and 415 nm; Beer's law is obeyed at both wavelengths over the range 20–320g of chloride. The best conditions for the spectrophotometric determination of chloride are determined and a procedure is recommended. Interferences from some of the most common anions are studied.

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Zusammenfassung Eine neue Methode für die Bestimmung von Chloridionen wurde angegeben. Sie beruht auf der Bildung von Chromylchlorid und dessen Extraktion mit Tetrachlorkohlenstoff. Der Extrakt hat spektrale Maxima bei 300 und 415 nm. Das Beersche Gesetz ist zwischen 20 und 320g Chlorid erfüllt. Die besten Bedingungen für die spektrophotometrische Bestimmung wurden ermittelt und ein Verfahren empfohlen. Störungsmöglichkeiten einiger üblicher Anionen wurden untersucht.

     

A First Insight in the Mechanisms Involved in the Self-Assembly of 2D-Hexagonal Templated SiO2 and TiO2 Mesostructured Films During Dip-Coating

Since mesoporous materials can be prepared by combining the sol-gel chemistry and the structuring effect of surfactants, they have attracted attention for application in various high technology fields. The present work deals with the analyses of the mechanisms involved in the formation of SiO₂ and TiO₂ highly organised 2D-hexagonal meso-structured films using Brij 58 as surfactant. The preparation of such films by dip-coating involves rapid evaporation which makes the different steps difficult to control. Simultaneous in-situ SAXS (synchrotron) and interferometry analyses have been performed to get a first understanding of the self-assembly process. SiO₂ and TiO₂ materials have a different chemical reactivity (kinetics and coordination aspects). However, we show that the mechanisms involved during dip-coating are quite similar : the self-assembly leading to the organised phase takes place at a final stage of the drying process, involves the formation of a disorganised intermediate phase and depends also on the presence of micellar interfaces in addition to film/air and film/substrate interfaces.