Synthesis and Characterization of Group 12 Metal(I) Complexes Bearing Extremely Bulky Boryl/Silyl Substituted Amide Ligands

Two extremely bulky boryl/silyl-substituted amide ligands, –N{B(DipNCH)₂}(SiR₃) (R = Me ^TBoL, R = Ph ^PhBoL; Dip = 2,6-diisopropylphenyl) were used in the preparation of the group 12 metal halide complexes, ^PhBoLZnBr, {^TBoLCd(μ-I)}₂, ^TBoLHgI, and ^PhBoLHgI. The reduction of these, and two previously reported compounds, ^PhBoLZnBr(THF) and {^PhBoLCd(μ-I)}₂, using a magnesium(I) compound, {(^MesNacnac)Mg}₂ (^MesNacnac = [(MesNCMe)₂CH]^–, Mes = mesityl), were carried out, leading to mixed results. In several cases these reactions led to decomposition, and deposition of the group 12 metal. However, in two instances the homobimetallic metal(I) complexes, ^TBoLM–M^TBoL (M = Zn or Hg), were isolated and crystallographically characterized. The reduction of {^PhBoLCd(μ-I)}₂ afforded the known cadmium(I) complex, ^PhBoLCd–Cd^PhBoL, but also gave a very low yield of the thermally unstable complex, ^PhBoLCd–Mg(THF)(^MesNacnac). The X-ray crystal structure of this compound reveals it to contain the first example of a Cd–Mg bond in a molecular compound.     

Fullerene-like (IF) Nb(x)Mo(1-x)S2 nanoparticles

IF-Mo1-xNbxS2 nanoparticles have been synthesized by a vapor-phase reaction involving the respective metal halides with H2S. The IF-Mo1-xNbxS2 nanoparticles, containing up to 25% Nb, were characterized by a variety of experimental techniques. Analysis of the powder X-ray powder diffraction, X-ray photoelectron spectroscopy, and different electron microscopy techniques shows that the majority of the Nb atoms are organized as nanosheets of NbS2 within the MoS2 host lattice. Most of the remaining Nb atoms (3%) are interspersed individually and randomly in the MoS2 host lattice. Very few Nb atoms, if any, are intercalated between the MoS2 layers. A sub-nanometer film of niobium oxide seems to encoat the majority of the nanoparticles. X-ray photoelectron spectroscopy in the chemically resolved electrical measurement mode (CREM) and scanning probe microscopy measurements of individual nanoparticles show that the mixed IF nanoparticles are metallic independent of the substitution pattern of the Nb atoms in the lattice of MoS2 (whereas unsubstituted IF-MoS2 nanoparticles are semiconducting). Furthermore the IF-Mo1-xNbxS2 nanoparticles are found to exhibit interesting single electron tunneling effects at low temperatures.     

A rapid and specific approach for direct measurement of pravastatin concentration in plasma by LC-MS/MS employing solid-phase extraction

A rapid, specific and sensitive LC-MS/MS assay using solid-phase extraction (SPE) for the determination of pravastatin, in human plasma is described. The plasma filtrate obtained after SPE, using a polymer base, a hydrophilic-lipophilic balance (HLB) cartridge, was submitted directly to short-column liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay, with negligible matrix effect on the analysis. For validation of the method, the recovery of the free analytes was compared with that from an optimized extraction method, and the analyte stability was examined under conditions mimicking the sample storage, handling, and analysis procedures. The extraction procedure yielded extremely clean extracts with a recovery of 107.44 and 98.93% for pravastatin and IS, respectively. The intra-assay and inter-assay precisions for the samples at the LLOQ were 3.30 and 7.31% respectively. The calibration curves were linear for the dynamic range 0.5-200 ng/mL with correlation coefficient r > or = 0.9988. The intra- and inter-assay accuracy ranged from 95.87 to 112.40%. The method is simple and reliable with a total run time of 3 min. This novel validated method was applied to the pharmacokinetic (PK) study in human volunteers receiving a single oral dose of 40 mg immediate release (IR) formulation.     

Rainbow Connection Number and Radius

The rainbow connection number, rc(G), of a connected graph G is the minimum number of colours needed to colour its edges, so that every pair of its vertices is connected by at least one path in which no two edges are coloured the same. In this note we show that for every bridgeless graph G with radius r, rc(G) ≤  r(r + 2). We demonstrate that this bound is the best possible for rc(G) as a function of r, not just for bridgeless graphs, but also for graphs of any stronger connectivity. It may be noted that for a general 1-connected graph G, rc(G) can be arbitrarily larger than its radius (K _1,n for instance). We further show that for every bridgeless graph G with radius r and chordality (size of a largest induced cycle) k, rc(G) ≤  rk. Hitherto, the only reported upper bound on the rainbow connection number of bridgeless graphs is 4n/5 ? 1, where n is order of the graph (Caro et al. in Electron J Comb 15(1):Research paper 57, 13, 2008). It is known that computing rc(G) is NP-Hard (Chakraborty and fischer in J Comb Optim 1–18, 2009). Here, we present a (r + 3)-factor approximation algorithm which runs in O(nm) time and a (d + 3)-factor approximation algorithm which runs in O(dm) time to rainbow colour any connected graph G on n vertices, with m edges, diameter d and radius r.     

Monophenylantimony(III) Derivatives of Cyclic Dithiocarbamates; Synthesis,Spectroscopic Characterization,and Antimicrobial Study

Abstract

Some new monophenylantimony(III) compounds having the formulas have been synthesized by reaction of phenylantimony(III) dichloride with the sodium salt of cyclic dithiocarbamates in 1:1 and 1:2 molar ratios. These newly synthesized compounds have been characterized by elemental analyses, molecular weight measurements, and their plausible structures have been proposed on the basis of IR, NMR (¹H and ¹³C), and ESI-mass studies. Sodium salts of cyclic dithiocarbamates and their corresponding organoantimony(III) derivatives (1–8) have been screened for antimicrobial activity against E. coli, P. aeruginosa (Bacteria) and A. niger and A. flavus (Fungi).     

Grafting onto Wool. IX. Graft Copolymerization of Vinyl Monomers by Use of Vanadium Oxyacetylacetonate as Initiator

Methyl methacrylate (MMA), acrylic acid (AAc), and vinyl acetate (VAc) were graft copolymerized onto Himachali wool in an aqueous medium by using vanadium oxyacetyl acetonate as initiator. Graft copolymerization was studied at 45, 55, 65, and 75°C for various reaction periods. The percentage of grafting was determined as functions of concentration of monomers, concentration of initiator, time, and temperature. The maximum percentage of grafting with each monomer occurred at 55°. Several grafting experiments were carried out in the presence of various additives which include HNO3, DMSO, and pyridine. Nitric acid was found to promote grafting of MMA. All these additives had adverse effects on grafting of VAc and AAc. MMA, VAc, and AAc were found to differ in reactivity toward grafting and followed the order MMA > AAc > VAc.     

Synthesis of C3-nitroalkylated-4-hydroxycoumarin and hydroxyiminodihydrofuroquinolinone derivatives via the Michael addition of cyclic 1,3-dicarbonyl compounds to β-nitrostyrenes

Herein, we describe a practical and efficient method for the C3-alkylation of 4-hydroxycoumarin by sonication under ‘on water’ conditions and mild temperatures using various substituted β-nitrostyrenes. In addition, we report on the development of a convenient process for the regioselective synthesis of angular hydroxyiminodihydrofuroquinolinone catalyzed by base. 4-Hydroxycoumarin and 4-hydroxy-1-methylquinolin-2(1H)-one reacted smoothly with various nitroolefins to furnish C3-nitroalkylated hydroxycoumarin derivatives (by sonication and ‘on water’ conditions) and hydroxyiminodihydrofuroquinolinone derivatives (ambient condition) as a mixture of Z (minor) and E (major) isomers, respectively. The mild reaction conditions employed, ease of isolation of the products and excellent yields constitute important features of the methodology.     

Effect of Donor-Acceptor Chromophores on Photophysical Properties of Newly Synthesized Pyrazolo-Pyrrolo-Pyrimidines (PPP)

Novel pyrazolo-pyrrolo-pyrimidine (PPP) derivatives having remarkable photophysical properties are designed with the help of theoretical semiempirical calculations. These compounds then synthesized successfully and studied effect of substituents on its photophysical properties.

Effect of Specific Solute-Solvent Interaction and Electron Donor-Acceptor Substituents of Novel Pyrazolo Naphthyridines on Fluorescence

Heterocyclic orthoaminoaldehyde such as 4-amino-3-(4-phenyl)-1-phenyl-1H-Pyrazolo[3,4-b]pyridine-5-carbaldehyde was synthesized by multistep reactions involving reduction of azido derivative 2 with LAH to yield aminoalcohol 3 and oxidation of it with MnO(2) to aminoaldehyde 4.The pyridine ring annulated on to 4 by Friedl?nder condensation using acetophenones in presence of base to obtained pyrazolo[3,4-h][1,6]naphthyridine 5 in excellent yield. Study of photophysical properties of 5 revealed that the absorption and emission of them depends up on the substituents present on benzene ring in newly annulated pyridine ring.     

Stochastic growth of cloud droplets by collisions during settling

In the last stage of droplet growth in clouds which leads to drizzle formation, larger droplets begin to settle under gravity and collide and coalesce with smaller droplets in their path. In this article, we shall deal with the simplified problem of a large drop settling amidst a population of identical smaller droplets. We present an expression for the probability that a given large drop suffers a given number of collisions, for a general statistically homogeneous distribution of droplets. We hope that our approach will serve as a valuable tool in dealing with droplet distribution in real clouds, which has been found to deviate from the idealized Poisson distribution due to mechanisms such as inertial clustering.