Total synthesis of (+)-xyloketal D, a secondary metabolite from the mangrove fungus Xylaria sp.

(+)-Xyloketal D was prepared in a one-pot multistep domino reaction by heating optically active 5-hydroxy-4-methyl-3-methylenepentan-2-one (R) in toluene with 2,4-dihydroxyacetophenone. The absolute configuration of the natural product was confirmed by preparation of the starting enone from a lactone of established absolute configuration.     

Effect of macropore convection on mass transfer in a bidisperse adsorbent particle

The importance of adsorption induced convection in the macropores of a bidisperse adsorbent particle is studied for a step change in mole fraction or total pressure at the surface of the particle. Material balance equations for a binary gas mixture are written for both the macropores and the macropores with allowance for convection in the macropores, which is described by Darcy's law. The coupled set o1' partial differential equations is solved by orthogonal collocation. The enhancement in mass transfer as a result of convection is assessed by comparing the fractional uptake curves obtained with and without allowance for convection. Both equilibrium-based and kinetic-based separation processes are considered. The effect of the presence of convection in determining the controlling diffusional resistance (macropore or micropore) is also examined. Due to inclusion of convection no single non-dimensional group alone can determine the relative importance of macropore and micropore resistances. Results show that convection can significantly affect the performance of an equilibrium-based macropore diffusion controlled process and that the enhancement in mass transfer is more for a particle with a high value of Darcy permeability.     

Synthesis and pharmacological activity of 4-(4'-(chlorophenyl)-4-hydroxypiperidine) derivatives

A new series of 4-(4'-chlorophenyl)-4-hydroxypiperidine derivatives (2-5), substituted at nitrogen, were synthesized and tested as potential analgesic compounds as well as evaluated for their effect on hypotensive activity. Results showed that all the derivatives exhibit significant analgesic activity in male Wistar rats at a dose of 50 mg/kg of body weight after intramuscular injection, when tested by thermal stimuli (tail flick test). Pethidine was used as reference drug. Compounds 2, 3 and 5 produced reduction in blood pressure in normotensive rat.     

Facile synthesis and characterization of monocrystalline cubic ZrO2 nanoparticles

Crystalline ZrO₂ nanoparticles were prepared from zirconium isopropoxide by slow hydrolysis and subsequent hydrothermal treatment of solutions containing various amounts of sodium hydroxide at 180 °C. Whereas moderately basic solutions lead to the formation of nanoparticles of monoclinic ZrO₂ with plate-like morphology, and nanoparticles of the cubic ZrO₂ high-temperature polymorph with diameters of approx. 5 nm were obtained from strongly basic solutions. The morphology, structure and properties of as-synthesized nanoparticles were characterized using HRTEM, XRD, Raman spectroscopy, UV–vis, PL spectroscopy and BET measurements. The formation of both, the monoclinic and the cubic polymorph, was confirmed by electron microscopy and Raman spectroscopy. The crystallinity and morphology of the resulting ZrO₂ nanoparticles can be adjusted by the choice of the reaction conditions. The cubic ZrO₂ nanoparticles have a high surface area (300 m²/g) and exhibit a strong photoluminescence in the UV region.     

Rotenoid and isoflavone metabolites from an antioxidant seed extract of Dalbergia lanceolaria subsp. paniculata (roxb.) thoth

Abstract

A new rotenoid named 12-O-methylrotenolol along with five known rotenoid and isoflavone metabolites were isolated from the seeds of Dalbergia lanceolaria subsp. paniculata, collected from Egypt. The structures of these compounds were identified by physical and spectroscopic data measurements ([α]_D, UV, 1D- and 2D-NMR and MS). The methanol extract of the seeds exhibited strong antioxidant activity with IC₅₀ value 0.7?µg/µl against DPPH radical, in respect to quercetin as antioxidant reference (IC₅₀ 1.5?μM), while the tested compounds from this extract showed weak activities with IC₅₀ values ranged from 19.6 to 33.0?µM.     

Blends of starch with ethylene vinyl alcohol copolymers: effect of water,glycerol, and amino acids as plasticizers

Blends of thermoplastic starch with poly(ethylene‐co‐vinyl alcohol) copolymer (EVOH) were melt extruded with water/glycerol as plasticizer and a series of amino acid additives. The biggest factor in end‐use mechanical properties proved to be the relative humidity (RH) during storage. Plasticized starch‐EVOH blends stored at 0 and 50% RH changed significantly over time, with, for example, the tensile strength (TS) of the glycerol‐plasticized blend increasing from 4.7 to 26.3 MPa over 8 weeks when maintained at 0% RH. In contrast, the TS of this same sample stored at 75% RH remained unchanged for 8 weeks. Amino acids provided relatively minor, but significant changes in mechanical properties with time. Based on TS, elongation‐to‐break, and modulus, it may be concluded that β‐alanine, sarcosine, and L ‐proline were more effective than glycerol at maintaining strong flexible blends. Increases in crystallinity and changes in morphology with time, as described by modulated DSC were correlated to these changes in mechanical properties. Published in 2007 by John Wiley & Sons, Ltd.     

Environmentally degradable bio-based polymeric blends and composites

Blends and composites based on environmentally degradable-ecocompatible synthetic and natural polymeric materials and fillers of natural origin have been prepared and processed under different conditions. Poly(vinyl alcohol) (PVA) was used as the synthetic polymer of choice by virtue of its capability to be processed from water solution or suspension as well as from the melt by blow extrusion and injection molding. Starch and gelatin were taken as the polymeric materials from renewable resources. The fillers were all of natural origin, as waste from food and agro-industry consisted of sugar cane bagasse (SCB), wheat flour (WF), orange peels (OR), apple peels (AP), corn fibres (CF), saw dust (SD) and wheat straw (WS). All the natural or hybrid formulations were intended to be utilized for the production of: a) Environmentally degradable mulching films (hydro-biomulching) displaying, in some cases, self-fertilizing characteristics by in situ spraying of water solutions or suspensions; b) Laminates and containers to be used in agriculture and food packaging by compression and injection molding followed by baking. Some typical prototype items have been prepared and characterized in relation to their morphological and mechanical properties and tested with different methodology for their propensity to environmental degradation and biodegradation as ultimate stage of their service life. A relationship between chemical composition and mechanical properties and propensity to biodegradation has been discussed in a few representative cases.     

Sorptive potential of sunflower stem for Cr(III) ions from aqueous solutions and its kinetic and thermodynamic profile

The sorptive potential of sunflower stem (180-300 μm) for Cr(III) ions has been investigated in detail. The maximum sorption (≥85%) of Cr(III) ions (70.2 μM) has been accomplished using 30 mg of high density sunflower stem in 10 min from 0.001 M nitric and 0.0001 M hydrochloric acid solutions. The accumulation of Cr(III) ions on the sorbent follows Dubinin-Radushkevich (D-R), Freundlich and Langmuir isotherms. The isotherm yields D-R saturation capacity X_m = 1.60 ± 0.23 mmol g⁻¹, β = −0.00654 ± 0.00017 kJ² mol⁻², mean free energy E = 8.74 ± 0.12 kJ mol⁻¹, Freundlich sorption capacity K_F = 0.24 ± 0.11 mol g⁻¹, 1/n = 0.90 ± 0.04 and of Langmuir constant K_L = 6800 ± 600 dm³ mol⁻¹ and C_m = 120 ± 18 μmol g⁻¹. The variation of sorption with temperature (283-323 K) gives ΔH = −23.3 ± 0.8 kJ mol⁻¹, ΔS = −64.0 ± 2.7 J mol⁻¹ K⁻¹ and ΔG_298k = −4.04 ± 0.09 kJ mol⁻¹. The negative enthalpy and free energy envisage exothermic and spontaneous nature of sorption, respectively. Bisulphate, Fe(III), molybdate, citrate, Fe(II), Y(III) suppress the sorption significantly. The selectivity studies indicate that Cr(III), Eu(III) and Tb(III) ions can be separated from Tc(VII) and I(I). Sunflower stem can be used for the preconcentration and removal of Cr(III) ions from aqueous medium. This cheaper and novel sorbent has potential applications in analytical and environmental chemistry, in water decontamination, industrial waste treatment and in pollution abatement. A possible mechanism of biosorption of Cr(III) ions onto the sunflower stem has been proposed.     

Synthesis and extraction properties of new chromogenic azo-calix[4]dibenzothiacrown ethers

Two novel chromogenic cone calix[4]dibenzothiacrown ethers 3 and 4 in which nitrophenylazo groups attached at the phenyl ring of dibenzothiacrown unit were described. The extraction properties of 3 and 4 toward different transition metal ions have been studied using conductometric technique and found to exhibit Cu²⁺ and Hg²⁺ selectivity with very high stability constants range from log K _assoc = 5.19 to log K _assoc = 8.72.     

Phosphodiesterase‐Inhibiting Glycosides from Symplocos racemosa

Phytochemical investigation of Symplocos racemosa resulted in the isolation of two new glycosides, symploracemoside ( 1 ) and symplomoside ( 2 ), which are structurally related to the reported benzoylsalireposide ( 3 ) and salireposide ( 4 ). The structure elucidation of the isolated compounds was based primarily on 1D‐ and 2D‐NMR analysis, including COSY, NOESY, HMQC, and HMBC correlations. These glycosides showed inhibitory activity against snake‐venom phosphodiesterase I.