CATALYSE INTRAMOLECULAIRE DE L'AMINOLYSE DES HETEROCYCLES PHOSPHORES DERIVES DES α AMINOAMIDES. II: ETUDE DE LA CYCLISATION DES PHOSPHORDIAMIDES INCORPORANT UN RESIDU DE β AMINOACIDE,REACTIVITE VIS A VIS DE NUCLEOPHILES DES HETEROCYCLES FORMES

Abstract

Derivatives of β aminoacids in form of esters 1 or nitrile 4 (table I) undergo in an alcohol-ate/alcohol medium a rearrangement (Fig. 2), with formation of a β peptide link, resulting in the formation of esters 6 (table II). According to the experimental conditions the six membered ring heterocycles 5 are detected or isolated. They are also synthetized by cyclisation of acids 2 or hydrazide 3 (Fig. 5). While phosphorus easily reacts with alcohols and water, leading respectively to esters 6 and acids 9 (Fig. 7), it remains unaffected by amines. These results are discussed in term of mechanisms of the phosphorylation. The applications for β peptide synthesis and the participation of the p amide group in phosphorylation are limited.     

Synthesis of green organogelators with a sulfide linkage via solvent-free Michael addition: soft templates for the preparation of size-controlled gold nanoparticles

Green organogelators with a sulfide linkage and free amino groups were synthesized via phase transfer catalysis using a N-benzylcinchonidinium bromide catalyst. Their self-assemblies in various common solvents were examined. These compounds exhibit high gelation ability especially in aromatic and highly polar solvents with a low critical gelation of 0.1 wt %. The organogels were analyzed by ¹H nuclear magnetic resonance (¹H NMR) and Fourier transfer-infrared spectroscopies (FT-IR), and their phase transition temperatures were determined by differential scanning calorimetry. The homogeneity of the gel networks was examined by field emission scanning electron microscopy and transmission electron microscopy (TEM). A lamellar structure was also confirmed by X-ray diffraction analysis. The organogels were employed as soft-templates for the in situ generation of stable gold nanoparticles dispersed in the gel matrix, and the resulting GNP dispersions were studied by ¹H NMR and UV–vis absorption. Transmission electron microscopy showed that GNPs assemble into a thin membrane-like structure.     

Electrodeposited copolymer electrolyte into nanostructured titania electrodes for 3D Li-ion microbatteries

The electrochemical synthesis of a copolymer electrolyte (PEO-PMMA) into titania nanotubes is described and studied. Compared with the electrochemical systems based on solid electrolytes deposited by top-down techniques, the copolymer/titania nanotube material reveals high electrochemical performance, opening new perspectives for the fabrication of 3D all-solid-state microbatteries.     

High Speed Video Camera and Electrical Signal Analyses of Arcs Behavior in a 3-Phase AC Arc Plasma Torch

A 3-phase AC plasma torch has been developed and aims at overcoming some limits of the classical DC torches in terms of efficiency, cost and reliability. However, the arc behavior in 3-phase plasma torch remains poorly explored. This paper is dedicated to the high speed video camera at 100,000 frames per second and electrical signal analyses of arcs behavior in a 3-phase AC arc plasma torch. First, a reference case at 150 A, in nitrogen as working gas, has been deeply analyzed. Afterwards, a parametric study based on current and inter-electrode gap has been carried out. Results show that only one arc can exist at a given time and arcs rotate by switching from a pair of electrodes to another one, following the maximal electrical gap potential. However, a particular “abnormal” arc behavior was sometimes observed. Indeed, the arc motion within the inter-electrode gap increases the heat exchange and stabilizes the 3-phase discharge whereas the system is unbalanced when the arc is in the periphery. The analysis highlights that the arc motion is strongly influenced by the electrode jet velocity and repulsive Lorentz forces. The parametric study shows that the current increases both jet velocity and arc discharge stability. Elsewhere, the increase of the inter-electrode gap can also stabilizes the electrical 3-phase arc discharge. Furthermore, the correlation between arc motion and current waveform is highlighted. This work is likely to open the way toward a better understanding of 3-phase discharges in the perspective of their further optimization.     

Tetraazamacrocycles lipophiles : synthese et application a l'extraction de Cu (II), Cd (II) et Pb (II)

The synthesis of three lipophilic n-dodecyl tetraazacycloalkanes is described. Extraction of Cu(II), Cd(II) and Pb(II) is related.     

Carbon nanotube synthesis in supercritical toluene

Multiwall carbon nanotubes (MWNTs) were synthesized in supercritical toluene at 600 degrees C and approximately 12.4 MPa using ferrocene, Fe, or FePt nanocrystals as growth catalysts. Toluene serves as both the carbon source for nanotube formation and the solvent. In contrast to vapor-phase synthetic routes, the supercritical solvent provides high precursor concentration and a homogeneous reaction environment with dispersed growth catalyst particles. Both carbon filaments and MWNTs are produced by this approach, and a growth mechanism is proposed to explain the factors that determine the nanotube versus filament morphology. The plasmon energies of the pi and pi + sigma valence electrons were measured using electron energy-loss spectroscopy (EELS) of individual carbon fibers and MWNTs as a characterization tool to complement the imaging data obtained from electron microscopy.     

Improving detector signal processing with pulse height analysis in Mössbauer spectrometers

A plenty of different programming techniques and instrument solutions are used in the development of Mössbauer spectrometers. Each of them should provide a faster spectrum accumulation process, increased productivity of measurements, decreased nonlinearity of the velocity scale, etc. The well known virtual instrumentation programming method has been used to design a computer-based Mössbauer spectrometer. Hardware solution was based on two commercially-available PCI modules produced by National Instruments Co. Virtual Mössbauer spectrometer is implemented by the graphical programming language LabVIEW 7 Express. This design environment allows to emulate the multichannel analyzer on the digital oscilloscope platform. This is a novel method based on Waveform Peak Detection function which allows detailed analysis of the acquired signal. The optimal treatment of the detector signal from various detector types is achieved by mathematical processing only. As a result, the possibility of an increase of signal/noise ratio is presented.     

Assignment of the 1H and 13C NMR Chemical Shifts of (3,4-Dihydro-2H-pyran-5-yl)-oxo-acetic Acid Methyl Ester Using the Two Dimensional HMBC Technique

The identification of (3, 4-dihydro-2H-pyran-5-yl)-oxo-acetic acid methyl ester has been realized by combination of two dimensional HETCOR and HMBC techniques. ¹³C and ¹H chemical shifts asignements are described.