Application of N,N‐bis(diphenylphosphino)aniline palladium(II) complexes as pre‐catalysts in Heck coupling reactions

Palladium(II) complexes with N,N‐bis(diphenylphosphino)aniline ligands catalyse the Heck reaction between styrene and aryl bromides, affording stilbenes in good yield. The structures of two of the complexes used as pre‐catalysts have been determined by single‐crystal X‐ray diffraction. Copyright © 2007 John Wiley & Sons, Ltd.     

Embedded diagonally implicit Runge–Kutta–Nystrom 4(3) pair for solving special second-order IVPs

In this paper, third-order 3-stage diagonally implicit Runge–Kutta–Nystrom method embedded in fourth-order 4-stage for solving special second-order initial value problems is constructed. The method has the property of minimized local truncation error as well as the last row of the coefficient matrix is equal to the vector output. The stability of the method is investigated and a standard set of test problems are tested upon and comparisons on the numerical results are made when the same set of test problems are reduced to first-order system and solved using existing Runge–Kutta method. The results clearly shown the advantage and the efficiency of the new method.     

The potential of serially coupled alkyl-bonded silica monolithic columns for high resolution separations of pharmaceutical compounds in biological fluids

Summary In this paper we investigate the potential of alkyl-bonded silica monolithic columns for the isolation and identification of drug-related components in biological fluids. Up to 6 columns have been connected in series to produce a chromatographic system with up to 40,000 plates. This high-resolution chromatography system has been coupled to both MS and NMR to enable efficient detection and characterisation of drug-related components in biological fluids. The use of six coupled columns has been shown to give enhanced resolution over a high quality silica particulate column packed with 3 μm material which exhibits the same back pressure. The effect of volume and mass load on the performance of monolithic columns for semi-preparative chromatography of biological fluids has also been investigated. In these studies it was possible to inject up to 100 mL of neat urine with no loss of chromatographic performance. Furthermore, upon re-testing, the columns showed similar chromatographic performance. Again several columns were serially connected, producing enhanced resolution in the semi-preparative mode.     

The anionic alkylation of easily reducible arenes. A photochemical route to nucleophilic aromatic substitution of anthracene by organolithiums

High yield nucleophilic addition ensues upon mixing tetrahydrofuran solutions of benzyllithium or cyclooctadienyllithium and anthracene at low temperatures At least part of this addition proceeds by a single electron transfer pathway. Photolysis of the resulting adducts leads to the elimination of lithium hydride, giving net nucleophilic substitution in approximately 50% yield. The analogous reaction fails with naphthalene, where photolysis of the organolithium/ arene mixture leads to dimeric products derived from the organolithium.     

Th,U and trace elements determination in Egyiptian Lake sediments by INAA and laser fluorimetry

A study was undertaken to determine element concentrations in Aswan High Dam Lake sediments. Sediment samples were collected from 40 to 500 km upstream of the dam to follow the sedimentation process and the distribution of Th, U and the trace elements in the lake. INAA was applied for the determination of Sm, Ce, Lu, Th, Cr, Yb, Au, Hf, Ba, Nd, Cs, Tb, Sc, Rb, Fe, Zn, Co, Eu, and Sb, while Laser Fluorimetry was applied for U determination. The accuracy and the reproducibility of the techniques were tested with IAEA standard materials (SL, Soil-7). The U values ranged from 4 ppm to 18 ppm, Th values were between 2 and 10 ppm, and showed a very good correlation with the rare earth elements and Fe. The distribution of most of the elements in the lake follows the same trend as the distribution of the clays in the sediments. Ba showed a negative correlation with most of the elements under investigation.Paper presented at the 3th International Conf. on Nuclear and Radiochemistry (NRC-3), Vienna, 1992.     

Analysis of tungsten-containing mixtures and some alloy steels by potentiometric titration methods

Reliable potentiometric titration methods are adopted for the analysis of tungsten mixtures analogous to some industrially important alloys such as low alloy tap steel, tungsten chisel, and high speed steels. Tungsten is separated as Hg₂WO₄ and unreacted Hg(I) is titrated with KBr. The techniques of oxidation with I₂ or reduction with KI and use of the selective arsenite reduction of Cr(VI) and/or Mn(IV) in the presence of V(V) or Fe(III) make it possible to determine alloy components without tedious separations. In all titrations the potential break is sharp enough for the precise establishment of the end point.     

Über Halogenphenylester der Phosphorsäure

A simple method for preparing halogenphenylesters of phosphoric, phenylphosphonic and phosphorous acid from the respective acid chlorides and phenols in the presence of various nitrogen-containing catalysts is described. Contrary to other methods, these reactions give high yields, despite of steric hindrance.