1H and 13C NMR Determination of the Enantiomeric Purity of Substituted 4-Amino-3- (thien-2-Yl)-Butyric Acids and 4-Amino-3-(Benzo[b]Furan-2-yl)-Butyric Acids,Ligands of the GabaB Receptor.

The enantiomeric composition and absolute configuration of 4-Amino-3-(benzo[b]furan-2-yl)-Butanoic Acids and of 4-Amino-3-(thien-2-yl)-Butanoic Acids 1 may be accurately determined by ¹H and ¹³C nuclear magnetic resonance analysis of the corresponding derivatives 3 prepared by reaction with chiral reagents. Correlation with HPLC is signaled.     

An inverse problem of the three-dimensional wave equation for a general annular vibrating membrane with piecewise smooth boundary conditions

This paper deals with the very interesting problem about the influence of piecewise smooth boundary conditions on the distribution of the eigenvalues of the negative Laplacian inR ³. The asymptotic expansion of the trace of the wave operator $\widehat\mu (t) = \sum\limits_{\upsilon = 1}^\infty {\exp \left( { - it\mu _\upsilon ^{1/2} } \right)} $ for small ?t? and $i = \sqrt { - 1} $ , where $\{ \mu _\nu \} _{\nu = 1}^\infty $ are the eigenvalues of the negative Laplacian $ - \nabla ^2 = - \sum\limits_{k = 1}^3 {\left( {\frac{\partial }{{\partial x^k }}} \right)} ^2 $ in the (x ¹,x ²,x ³), is studied for an annular vibrating membrane Ω inR ³ together with its smooth inner boundary surfaceS ₁ and its smooth outer boundary surfaceS ₂. In the present paper, a finite number of Dirichlet, Neumann and Robin boundary conditions on the piecewise smooth componentsS ^* _i(i=1, …,m) ofS ₁ and on the piecewise smooth componentsS ^* _i(i=m+1, …,n) ofS ₂ such that $S_1 = \bigcup\limits_{i = 1}^m {S_i^* } $ and $S_2 = \bigcup\limits_{i = m + 1}^n {S_i^* } $ are considered. The basic problem is to extract information on the geometry of the annular vibrating membrane ω from complete knowledge of its eigenvalues by analyzing the asymptotic expansions of the spectral function $\widehat\mu (t)$ for small ?t?.     

Ruthenium(II) 2-hydroxybenzophenone N(4)-substituted thiosemicarbazone complexes

New ruthenium(II) complexes with 2-hydroxybenzophenone N(4)-substituted (Me, Ph and/or piperidyl) thiosemicarbazones have been prepared and characterised by elemental analysis, molar conductivity, thermal analysis, spectroscopy (i.r., ¹H-n.m.r. and u.v.–vis.) and by cyclic voltammetry. The thiosemicarbazones coordinate to ruthenium(II) as mononegative tridentate ligands via the deprotonated hydroxyl group, N¹ nitrogen and thione sulphur centres. The redox properties, nature of the electrode processes and the stability of the complexes towards oxidation in CH₂Cl₂ are discussed. The change in the E _1/2 values of the complexes can be related to the basicity of the N(4)-substituents. All the complexes display an irreversible one-electron charge-transfer couple in the potential range studied. This revised version was published online in June 2006 with corrections to the Cover Date.     

Structure and stability characteristics of turbulent planar flames with inhomogeneous jet in a concentric flow slot burner

Turbulent flames with compositionally inhomogeneous mixtures are common in many combustion systems. Turbulent jet flames with a circular nozzle burner were used earlier to study the impact of inhomogeneous mixtures, and these studies showed that the nozzle radius affects the flame stability. Accordingly, planar turbulent flames with inhomogeneous turbulent jet are created in a concentric flow slot burner (CFSB) to avoid this effect in the present study. The stability characteristics, the mixing field structure, and the flame front structure were measured, and the correlations between stability and the mixing field structure were investigated. The mixture fraction field was measured in non-reacting jets at the nozzle exit using highly resolved Rayleigh scattering technique, and the flame front was measured in some selected turbulent flames using high-speed Planar Laser-Induced Fluorescence (PLIF) of OH technique. The data show strong correlations between flame stability and the range of mixture fraction fluctuations. The flames are highly stabilized within a mixing field environment with the range of fluctuation in mixture fraction close to the range of the flammability limits. The mixing field structure is also illustrated and discussed using a mixing regime diagram and showed that the scatter of the data of the different cases is consistent with the classified mixing regimes. Lean flames are stabilized in the current slot burner. The flame front structure topology varies consistently from thin, small curvature at the low level of turbulence and higher equivalence ratio to more wrinkled, larger curvature, but a thicker structure at a higher level of turbulence and lower equivalence ratio.     

Effect of sulphate groups on catalytic properties of chromium supported by zirconia in the <Emphasis Type="Italic">n</Emphasis>-hexane aromatization

Catalysts based on chromium supported by sulphated and unsulphated zirconia have been synthesised, in one step, by sol–gel method and dried in hypercritical solvent conditions. Comparative study of their catalytic properties shows that dispersed Cr³⁺ seems to be the active species in the n-hexane aromatisation reaction. However, the acidity generated by sulphate groups acts as coke eliminator of the layers deposed on the surface mainly when catalyst is calcined at high temperature.     

Studies on pyrrolidinones. Synthesis of 1,2,3,5,11,11a-hexahydroindolizino[7,6-b]indole-3,11-dione

Condensation of N-trimethylsilylindole with methyl N-trimethylsilyloxymethylpyroglutamate is the best method to obtain methyl N-indolylmethylpyroglutamate. Friedel-Crafts cyclization of the corresponding acid yields a new ketone (1,2,3,5,11,11a-hexahydroindolizino[7,6-b] indole-3,11-dione).     

Mixed-ligand complexes of copper(I) with diimines and phosphines: Effective catalysts for the coupling of phenylacetylene with halobenzene

New copper(I) mixed-ligand complexes 1–4 of the formula Cu(N–N)PR₃X, where N–N = 1,10-phenanthroline (phen), 2,2′-bipyridine (bpy), 5,5′-dimethyl-2,2′-bipyridine (5,5′dimbpy) and PR₃ = tricyclohexylphosphine, tris(2-cyanoethyl)phosphine and isopropyldiphenylphosphine, have been synthesized. The complexes were characterized by EA, IR, NMR and single crystal X-ray diffraction. The solution fluorescence emission spectra were measured. The single crystal X-ray analysis showed that the copper(I) ion is four-coordinate with a distorted tetrahedral geometry. The complexes catalyze the formation of diphenylacetylene from the coupling of halobenzene with phenylacetylene. The complex Cu(5,5′-dimethylbpy)P{(cyhexyl)₃}I showed the highest catalytic activity. At room temperature all four complexes exhibit, in dichloromethane, emission maxima in the 329–344 nm range, corresponding to intra-ligand excited states.     

Solid-phase extraction of Pb2+ ion from environmental samples onto L-AC-Ag-NP by flame atomic absorption spectrometry (FAAS)

The development of a solid-phase extraction (SPE) procedure for the pre-concentration of trace amounts of Pb²⁺ ion on 2-furan-2-yl-1-furan-2-ylmethyl-1H-benzoimidazole loaded on activated carbon modified with silver nanoparticles (L-AC-Ag-NP) was presented. The metal ion retained on the sorbent was quantitatively determined via complexation with the ligand. The complexed metal ion was efficiently eluted using 10 mL of 4 mol L^?1 sulphuric acid in 10 w/v% acetone. The influences of the analytical parameters, including pH, amounts of the ligand and the solid phase, eluent conditions and sample volume, on the recoveries of the metal ion were optimised. Using the optimised parameters, the linear response of the SPE method for Pb²⁺ ion were in the ranges of 0.2–160 µg L^?1, and the detection limit for Pb²⁺ ion was 0.034 µg L^?1. The proposed method exhibits a pre-concentration factor (PF) of 80 and an enhancement factor of 30 for Pb²⁺ ion. The presented results demonstrate the successful application of the proposed method for the determination of Pb²⁺ ion in some real samples with high recoveries (>93%) and reasonable relative standard deviation (RSD < 2%).