Novel method for the synthesis of 1,2,4‐oxadiazoles using alumina supported ammonium fluoride under solvent‐free condition

Alumina supported ammonium fluoride was found as an efficient reagent for the synthesis of 1,2,4‐oxadi‐azoles of amidoximes under solvent free conditions using microwave irradiation. This method is a one‐pot, easy, rapid, and high‐yielding reaction for the synthesis of 1,2,4‐oxadiazole derivatives from amidoximes and acyl chlorides. Reaction of amidoximes with acylchlorides in the presence of alumina without ammonium fluoride gave only the corresponding O‐acylamidoximes as major product.     

The preparation of quinolines and related fused-ring heterocycles from the dianions of benzoylacetone,certain cyclic ketone oximes,or certain substituted hydrazones

C(α),O-Dilithiooximes, C(α),N-dilithiobenzoylhydrazones, or C(α),N-dilithiocarboalkoxyhydrazones were prepared in an excess of lithium diisopropylamide (LDA) and condensed with 2-aminobenzophenones, or isatoic anhydrides to give intermediates that were treated with aqueous acid, which caused their hydrolysis, cyclodehydration and/or linear dehydration to give products which were substituted quinolines or related fused-ring heterocycles (e.g., cycloheptaquinolines). Dilithiobenzoylacetone was condensed with 2-aminobenzophenones, which was followed by acid cyclodehydration to substituted 2-phenacylquinolines.     

Preparation of Polycarbonate-ZnO Nanocomposite Films: Surface Investigation after UV Irradiation

Polycarbonate (PC)-ZnO films with different percentages of ZnO were prepared by a solution stirring technique and subjected to ultraviolet (UV; λ = 254 nm) irradiation. Structural parameters of the samples and the effects of UV irradiation on the surface properties of the PC and PC-ZnO nanocomposites were evaluated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), water contact angle (WCA) measurements, and a Vickers microhardness (H_V) tester. The XRD patterns of the nanocomposite films were found to show an increase in crystallinity with the increasing ZnO nanoparticles percentage. The WCA was found to be reduced from 90° to 17° after 15 h of UV irradiation, which could be ascribed to the oxidation of the surface of the samples during the irradiation and exposure of the ZnO nanoparticles, a result that is also supported by the obtained XPS data. The microhardness value of the PC-ZnO films including 30 wt.% ZnO enhanced considerably after UV radiation, which can also be attributed to the exposition of the ZnO nanoparticles after photodegradation of the PC superficial layer of the nanocomposite films.     

INTERACTION BETWEEN ADSORPTION LAYERS OF MACROMOLECULES

Stability and rheological properties of concentrated emulsions (including those for manufacture of vitamin microcapsules) can be related to elementary coalescence acts and adhesion of emulsion drops interacting through thin layers (microscopic emulsion films) of a dispersion medium

A new procedure was used for measuring the adhesion force f_a between two drops of n-heptane in polymer solutions and lifetime τ of the drops in the contacts depending on the volume concentration C of the polymer, time of formation t_f of adsorption layers, temperature T, capillary pressure P_c in the film, surface area S of the film, and on addition of acetone and tannin. The molecular mechanism of the interaction between adsorption layers of polymers and of the process of film destruction is discussed on the basis of the relationships obtained for interaction free energy Δ F_a, activation energy E, destruction activation volume δ and physico-chemical parameters.     

A peptide bromoiodinane approach for asymmetric bromolactonization

A series of 37 peptides containing an iodo-aryl amide active site were generated by means of both solid phase and conventional synthesis. These peptides were screened for asymmetric induction in the bromolactonization of 4-phenyl-4-pentenoic acid based on the generation of chiral bromoiodinane bromenium sources. The study culminated in the discovery of a tri-peptide iodo-aryl amide that effected the desired bromolactonization in quantitative conversion with 24% ee. The experiments disclosed herein provided valuable insight that ultimately facilitated the development of more synthetically useful enantioselective halocyclization methodology.     

7-β- and 10-β-Hydroxylated congeners of CAF-603; elucidation of absolute configuration of CAF-603 family,and their SAR studies in the anti-fungal activity

Novel 7-β- and 10-β-hydroxylated congeners of CAF-603 (4 and 5, respectively) were isolated from Trichoderma crassum. Relative configuration of 4 was determined by NOE experiments. Stereochemistry of 7-β-hydroxy group in 5 was established by a combination of vicinal ³J_H–H analyses and quantum chemical calculations. Absolute configurations of 4 and 5 were established by observing the Cotton effects of their bis(2-naphthoate) esters. T. crassum also produce known CAF-603 (1), 14-hydroxy and 8,9-β-epoxy derivatives (2 and 3, respectively). Present study first established the absolute configuration of CAF-603 family by taking their biosyntheses into account. Preliminary biological experiments revealed that the molecular target strictly recognizes the β-side of the cycloheptane ring.     

A Proline-Based Aminophosphinic Acid Ligand and It’s Vanadyl Complex: Synthesis,Characterization and In Vitro Inhibitory Effects on α-Amylase And α-Glucosidase

Abstract

A proline-based aminophosphinic acid ligand and it's vanadium complex have been synthesized and characterized by spectroscopic techniques. The inhibitory activity on pancreatic α-amylase and Baker's yeast α-glucosidase has been examined in vitro. The novel complex showed more inhibitory potency against pancreatic α-amylase and Baker's yeast α-glucosidase compared to acarbose as an antidiabetic drug.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Kinetics of the Initial Stage of Gelation in Chitosan Solutions Containing Glutaric Aldehyde: Viscometric Study

The effects of glutaric aldehyde concentration C _GA(in the range from 0.07 to 0.2 wt %) and temperature T(from 20 to 65°C) on the kinetics of an increase in the effective viscosity _effof aqueous solutions of chitosans (C _CH= 2.4 wt %, pH 3.6, and ionic strength I= 0.05) with molecular masses equal to 33 × 10⁴and 55 × 10⁴and the degrees of substitution at N-acetyl and amino groups of 0.08 and 0.90, respectively were studied. The kinetic curves _eff(t) exhibited the induction periods of a relatively slight increase in the viscosity of chitosan–glutaric aldehyde mixed solutions with time followed by the periods of a drastic increase in the viscosity. The former periods correspond to the formation of gel clusters; the latter periods, to the gelation over the whole volume of a solution. Optimal ranges of the parameters C _GAand Twere determined for the preparation of spherical gel particles of slightly cross-linked chitosan, which are used for the sorption of heavy metals from low-concentrated solutions.