Synthesis of trideuteratedO-alkyl platelet activating factor and lyso derivatives

Racemic heavy isotope analogs of 1-O-alkyl-sn-glycero-3-phosphocholine (lysoPAF) and 1-O-alkyl-2-O-acetyl-sn-glycero-3-phosphocholine (PAF) were prepared for use as internal standards to facilitate quantitative studies based on mass spectrometry. Starting from pentadencane-1,15-diol andrac-glycerol-1,2-acetonide, a convergent synthesis of 1-O-[16′-²H₃]hexadecyl and 1-O-[18′-²H₃]octadecylrac-glycero-3-phosphocholine and their acetyl derivatives is described. Three deuterium atoms were introduced at the terminal position of the 1-O-alkyl group by displacement of thep-toluensulfonyl group from 1-O-alkyl-15′-p-toluensulfonate and 1-O-alkyl-17′-p-toluensulfonate with [²H₃]-methylmagnesium iodide. The 1-O-alkyl-17′-p-toluensulfonate was obtained by reaction of the 1-O-alkyl-15′-p-toluensulfonate with allylmagnesium bromide, followed by reductive ozonolysis and treatment withp-toluenesulfonyl chloride. The hydroxyl group at C-2 was protected by a benzyl group and removed at a late stage in the synthesis. This provided the corresponding lysoderivatives or allowed preparation of racemic PAF by subsequent acetylation of the free hydroxy group. The phosphocholine moiety was introduced at glycerol C-3 by reaction with bromoethyldichlorophosphate and trimethylamine. The synthetic compounds were analyzed by FAB/MS and GC/NICIMS. They were shown to contain less than 0.6% protium impurity.     

Adhesion Science and Surface Analysis. Typical Examples

A number of surface modification methods using mechanical, chemical, electrochemical or physical processes have commonly been employed to treat adherend surfaces and improve adhesion in various bi- or multi-layered systems which play a key role in many advanced technologies. Results reported in this review paper deal more particularly with components of polymer-metal systems and provide typical examples of surface analysis obtained by x-ray photoelectron spectrometry (XPS), ion scattering spectrometry (ISS), low-energy electron induced x-ray spectrometry (LEEIXS), optically stimulated electron emission (OSEE) and Fourier transform infra-red spectrometry (FTIR). These examples concern, on the one hand, metallic adherends (aluminum, stainless steel, zinc-coated steel, gold) the surfaces of which were modified by cleaning, etching, oxidation, conversion or chemical grafting and, on the other hand, bonded joints (polyester-steel and epoxy-aluminum systems) which were delaminated using a peel test and a three-point flexure test, respectively.     

Copper‐Catalyzed C–N,C–O Coupling Reaction of Arylglyoxylic Acids with Isatins

The copper(II)‐catalyzed decarboxylative coupling reactions of arylglyoxylic acids with isatins afford 4H‐benzo[d][1,3]oxazin‐4‐ones via decarbonylation and concurrent C–N, C–O bond formation.

     

Antifungal,antiaflatoxin and antioxidant potential of chemically characterized Boswellia carterii Birdw essential oil and its in vivo practical applicability in preservation of Piper nigrum L. fruits

The study explores the chemical profile, antimicrobial and antioxidant activity of Boswellia carterii essential oil (EO). The EO significantly inhibited growth and aflatoxin production by the food borne toxigenic strain of Aspergillus flavus at 1.75 μl/ml and 1.25 μl/ml respectively. It exhibited broad fungitoxic spectrum against 12 food borne moulds and also showed strong antioxidant activity, IC₅₀ value and % inhibition of linoleic acid peroxidation being 0.64 μl/ml and 51.68% respectively. The antifungal action of EO was observed in terms of reduction in ergosterol content of plasma membrane of A. flavus. As fumigant in food system in storage containers, the EO provided 65.38% protection against fungal deterioration of Piper nigrum. GC–MS results revealed 31 components of EO. The chemically characterized B. carterii EO may thus be recommended as plant based preservative in view of its antifungal, antiaflatoxigenic, antioxidant activity and efficacy in food system.     

An investigation of the flocculation characteristics of polyacrylamide‐grafted chitosan

To investigate the flocculation characteristics of polyacrylamide (PAM)‐grafted chitosan, a series of PAM‐grafted chitosan copolymer (Chito‐g‐PAM1 to Chito‐g‐PAM4) have been synthesized by ceric ammonium nitrate‐induced solution polymerization technique in nitrogen atmosphere. The flocculation characteristics of the polymer samples (PAM, grafted and ungrafted chitosan) were studied by settling test and jar test methods in the colloidal suspensions of kaolin, iron ore, silica, and bentonite powder. It was found that the settling performance of Chito‐g‐PAM3 is best among the polymer samples. The jar test results indicate that the ungrafted chitosan has better water clarifying performance than both the PAM and grafted chitosan. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Phosphotungstic Acid: An Efficient Catalyst for the Aqueous Phase Synthesis of Bis-(4-hydroxycoumarin-3-yl)methanes

In this present work, we report that phosphotungstic acid provides a simple, efficient and environmentally benign route is a two-component one-pot domino Knoevenagel-type condensation/Michael reaction between 4-coumarin derivative and an aldehyde in water as a solvent in shorter duration with high yields.      

Resistive switching memory characteristics of Ge/GeOx nanowires and evidence of oxygen ion migration

The resistive switching memory of Ge nanowires (NWs) in an IrO_x/Al₂O₃/Ge NWs/SiO₂/p-Si structure is investigated. Ge NWs with an average diameter of approximately 100 nm are grown by the vapor–liquid-solid technique. The core-shell structure of the Ge/GeO_x NWs is confirmed by both scanning electron microscopy and high-resolution transmission electron microscopy. Defects in the Ge/GeO_x NWs are observed by X-ray photoelectron spectroscopy. Broad photoluminescence spectra from 10 to 300 K are observed because of defects in the Ge/GeO_x NWs, which are also useful for nanoscale resistive switching memory. The resistive switching mechanism in an IrO_x/GeO_x/W structure involves migration of oxygen ions under external bias, which is also confirmed by real-time observation of the surface of the device. The porous IrO_x top electrode readily allows the evolved O₂ gas to escape from the device. The annealed device has a low operating voltage (<4 V), low RESET current (approximately 22 μA), large resistance ratio (>10³), long pulse read endurance of >10⁵ cycles, and good data retention of >10⁴ s. Its performance is better than that of the as-deposited device because the GeO_x film in the annealed device contains more oxygen vacancies. Under SET operation, Ge/GeO_x nanofilaments (or NWs) form in the GeO_x film. The diameter of the conducting nanofilament is approximately 40 nm, which is calculated using a new method.     

Exceptionally High Dielectric Constant in Ceramic Pr2CuO4

The pristine layered cuprate Pr₂CuO₄ samples of >95% density were fabricated as thin disks. The samples, analyzed by X‐ray diffraction and Scanning electron microscopy, showed clean T′‐type phase with Rietveld refined lattice parameters a = b = 3.95805(±5) Å and c = 12.2262(±5) Å. The measured dielectric properties of the Pr₂CuO₄ ceramics, in the temperature range ?100°C–150°C and frequencies (ν) 0.1 Hz–1 MHz, showed extremely high ε_r′ > 10⁴ (above ?30°C), and dissipation (tan δ = ε_r′′/ε_r′) between 0.1 and 5 (for 500 Hz ≤ ν ≤ 1 MHz, and ?100 ≤ T ≤ 150°C). The ac conductivity of Pr₂CuO₄ ceramics ranged between 10^?6 and 10^?3 Scm^?1 for the measured frequencies and temperatures, and showed frequency‐dependent double power law behavior akin to a modified Jonscher's power law.     

Structural,magnetic, and textural properties of iron oxide-reduced graphene oxide hybrids and their use for the electrochemical detection of chromium

Superparamagnetic Fe₃O₄ nanoparticles were anchored on reduced graphene oxide (RGO) nanosheets by co-precipitation of iron salts in the presence of different amounts of graphene oxide (GO). A pH dependent zeta potential and good aqueous dispersions were observed for the three hybrids of Fe₃O₄ and RGO. The structure, morphology and microstructure of the hybrids were examined by X-ray diffraction, transmission electron microscopy (TEM), Fourier transform infrared spectroscopy, Raman and X-ray photoelectron spectroscopy. TEM images reveal lattice fringes (d₃₁₁ = 0.26 nm) of Fe₃O₄ nanoparticles with clear stacked layers of RGO nanosheets. The textural properties including the pore size distribution and loading of Fe₃O₄ nanoparticles to form Fe₃O₄–RGO hybrids have been controlled by changing the concentration of GO. An observed maximum (～10 nm) in pore size distribution for the sample with 0.25 mg ml^?1 of GO is different from that prepared using 1.0 mg ml^?1 GO. The superparamagnetic behavior is also lost in the latter and it exhibits a ferrimagnetic nature. The electrochemical behavior of the hybrids towards chromium ion was assessed and a novel electrode system using cyclic voltammetry for the preparation of an electrochemical sensor platform is proposed. The textural properties seem to influence the electrochemical and magnetic behavior of the hybrids.     

Iron(III)-mediated ATRP systems of n-docosyl acrylate with AIBN and BPO

Well-defined poly(n-docosyl acrylate) (PDA) with narrow molecular weight distribution has been synthesized by atom transfer radical polymerization (ATRP) and reverse ATRP of n-docosyl acrylate (DA) at 80 °C in N,N-dimethylformamide using the carbon tetrabromide/FeCl₃/2,2′-bipyridine (bpy) initiation system in the presence of 2,2′-azobisisobutyronitrile (AIBN) and benzoyl peroxide (BPO) as the source of reducing agent. The rates of polymerization for both the systems exhibit first-order kinetics with respect to the monomer, however, peroxide-initiated system shows slow rate of polymerization as compared to the azo-system. The effect of various reaction parameters on number average molecular weight (M _n ) and molecular weight distribution (M _w/M _n ) have been investigated. The resulting PDA that obtained in presence of AIBN and BPO systems has been compared for both the conventional and reverse ATRP. The reverse ATRP initiated by peroxides behaves differently than that of the azo initiators. In reverse ATRP with BPO, the rate of polymerization (R _p) has been significantly increased with the increase of BPO resulting higher M _n and broader M _w/M _n . The reverse ATRP of DA did not exhibit living characteristics with BPO system. PDA has been characterized by GPC, FTIR, and NMR spectroscopy.