Catalytic applications of nano β-PbO in Paal-Knorr reaction

Several 2,5-dimethyl-N-substituted pyrroles were prepared by the condensation of different substituted anilines with 2,5- hexanedione using nano lead oxide as an efficient and recyclable catalyst.All the synthesized compounds are confirmed through IR, ¹H NMR,¹³C NMR and mass spectral data.Nano lead oxide β-PbO（P85） was prepared by dissolving lead acetate dihydrate in 1- propanol at a pH 9.0 under stirring at 85℃.The structural study and surface morphology of the lead oxide（PbO） were characterized using X-ray diffraction（XRD）,Scanning electron microscopy（SEM） and the functional groups of the PbO sample were investigated using infrared spectrophotometer.     

Asymmetric Mannich reaction catalyzed by N-arylsulfonyl-l-proline amides

Proline-derived N-sulfonylcarboxamides efficiently catalyze the asymmetric Mannich reaction of cyclic ketones with N-(p-methoxyphenyl)-protected iminoglyoxylate. Both classical organic solvents and ionic liquids were used as the reaction media. With cyclohexanone, the reaction proceeded with high enantioselectivity (99% ee). Enamine intermediates were investigated by DFT calculations.     

Using Single-Channel Blind Deconvolution to Choose the Most Realistic Pharmacokinetic Model in Dynamic Contrast-Enhanced MR Imaging

In dynamic contrast-enhanced magnetic resonance imaging, there has been no consensus in the choice of the pharmacokinetic model. In this paper, a new approach for assessment of the most realistic model for a given tissue is presented. Non-blind and single-channel blind deconvolution algorithms were used in quantitative magnetic resonance dynamic contrast-enhanced imaging of the mouse masseter muscle to compare the realism of two different pharmacokinetic models for the tissue residue function. The first was the adiabatic approximation tissue homogeneity model (aaJW) and the second, the two-compartment exchange model (2CXM). Normals and mice treated with the substance C48/80 were studied. C48/80 increases both blood flow and contrast leakage in muscle substantially. The obtained approximation accuracy was evaluated for both pharmacokinetic models. In addition, the arterial input functions (aifs) estimated using blind deconvolution were compared to the corresponding observed aifs. The hypothesis is that the most realistic model of the tissue residue function leads to the best fits. The non-blind deconvolution did not result in any clear answer. For blind deconvolution, the aifs of the aaJW model were very similar to the corresponding observed aifs, and clearly more so than the aifs of the 2CXM model. Also, the approximation of the observed tracer time sequences was more accurate for the aaJW than the 2CXM model. The realism of different pharmacokinetic models in describing the passage of a tracer through a microvascular bed of a single tissue could be assessed using single-channel blind deconvolution.     

Alternatively modified bingel reaction for efficient syntheses of C60 hexakis-adducts

It was found that the C60 hexakis-adduct (Th) bearing 12 electron-donating N,N-dimethylaniline moieties could not be synthesized by the Bingel-Hirsch method with either classical or deviated experimental parameters in a one-pot reaction. A different modification to the original Bingel reaction without the use of any templating agent was necessary for high-yield synthesis of the compound. The generalization of this alternatively modified Bingel method to the preparation of other C60 hexakis-adducts is demonstrated. [structure: see text].     

Synthesis of C15-C27 segment of venturicidine X by utilizing desymmetrization protocol

We have achieved the synthesis of C15-C27 fragment of venturicidine X using desymmetrization protocol, substrate-controlled Grignard reaction, Barton-McCombie reaction, Sharpless epoxidation, and TBSOTf-mediated rearrangement to produce the aldol product through a non-aldol route as the key step following 23 longest linear sequences with 6.4% overall yield starting from a known intermediate 11.     

Carbon paste electrodes modified with Bi(2)O(3) as sensors for the determination of Cd and Pb

Carbon paste electrodes bulk-modified with Bi(2)O(3)were used for the determination of Cd(II) and Pb(II). The best composition was 1% (wt%) Bi(2)O(3) in the paste. The measurements were made by differential pulse voltammetry in the potential range from -1.2 V to -0.3 V. The peak potential of the reoxidation of Cd is -0.85 V, and of Pb -0.60 V vs. SCE. The lowest concentration that could be determined was 5 microg L(-1) of both metals (preconcentration time 240 s), the relative standard deviation was 3.5%-5.0% (four determinations). The correlation coefficient ( r(2)) of the calibration curves was 0.9966 (for Cd) and 0.9971 (for Pb). The Bi(2)O(3)-modified electrode could be used for the analysis of drinking water, mineral water and urine.     

Structural,optical and photoelectron spectroscopic studies of nano/micro ZnO:Cd rods synthesized via sol-gel route

Thin films of cadmium doped zinc oxide rod like microstructure have been synthesized by a very simple sol-gel dip coating technique. Sols were prepared from hydrated zinc oxide precursor and 2-methoxyethanol solvent with monoethanolamine as a sol stabilizer. XRD pattern confirmed the hexagonal wurtzite structure of the deposited ZnO films. Surface morphologies of the films have been studied by a scanning electron microscope and an atomic force microscope, which confirmed that the films are composed of densely packed randomly oriented nano/submicron rods with diameter in the range 300–400 nm having various lengths. We proposed a possible growth mechanism for this rodlike structure. X-ray photoelectron spectroscopic study was used to determine the binding energies and the Zn 2p3/2, Cd 3d5 and O 1s peaks in the XPS spectra were located at 1021.08 eV, 404.6 eV and 529.8 eV respectively, which confirmed the Cd doping in ZnO. Cadmium content in the film was estimated both from energy dispersive X-ray analysis and XPS measurement. Band gap energy determined from optical transmittance spectra systematically varied from 3.28 eV to 3.15 eV for 0% to 5.6% of Cd doping. Urbach parameter determined from the band tail of the transmittance spectra showed that it increased with doping percentage and this parameter for a fixed cadmium doping level decreased with increase of temperature.     

Determination of 99Tc in bentonite clay samples using inductively coupled plasma mass spectrometry

A method was developed for the determination of ⁹⁹Tc at low concentrations in clay samples. The chemical treatment of the samples prior to chemical separation and analysis comprised leaching with sulphuric acid/ sodium bromate. After leaching, pertechnetate was extracted with Alamine-336/chloroform and then back-extracted into nitric acid. Detection was carried out using inductively coupled plasma mass spectrometry, ICP-MS. The instrumental detection limit was 0.45 pg/mL, which corresponds to 0.28 mBq/mL. With the use of a desolvating nebuliser, the detection limit was lowered by about a factor of five. The results were compared with a method using radiometric detection. Received: 16 April 1998 / Revised: 12 June 1998 / Accepted: 16 June 1998     

Voltammetric determination of 2-mercaptobenzothiazole in a mixture of ethylene glycol + water

Voltammetry employing rotating platinum and disc electrodes proves to be a suitable method for determining 2-mercaptobenzothiazole in the mixture ethylene glycol + water in the relatively large concentration range 0.005–1% (i.e. approximately 3 × 10^?4 ?6 × 10^?2 mol 1^?1).The shapes of the voltammetric curves of thiol on both electrodes are essentially identical. During the gradual anodic polarization of the electrodes thiol is oxidized to a disulphide and adsorbed on the electrode surface, which is not accompanied by a conspicuous peak. In the more positive regions of the potential the next anodic process takes place:

manifested by the formation of an anodic peak.The calibration graphs are based on the linear dependence of the current of anodic peak I_A on the thiol concentration.In all cases the use of the rotating platinum electrodes proves to be more advantageous. The results are time reproducible, the determination requires no treatment of samples and requires approximately 15 min.