A novel (E,E)-dioxime and its mono-, di- and trinuclear complexes bearing tetradentate octyl sulfanyl phenylamino substituents. Synthesis,characterization and electrochemical properties of its transition metal complexes

A new vic-dioxime, 13,14-bis-(hydroxyimino)-9,12,15,18-diazadithiaoctacosane, has been synthesized from 2-octylsulfanylaminobenzene and (E,E)-dichloroglyoxime. Mononuclear transition metal complexes of Ni^II, Cu^II, Co^II and Fe^II have been prepared and were found to have a metal–ligand ratio of 1:2. The synthesis of di- and trinuclear complexes was achieved with U^IVO₂ and Cu^II depending on the stoichiometry of the reactants. The complexes were characterized by elemental analysis, ¹H-n.m.r., u.v.–vis, i.r., f.a.b.-m.s. and by cyclic voltammetry.     

A new affinity-HPLC packing for protein separation: Cibacron blue attached uniform porous poly(HEMA-<Emphasis Type="Italic">co</Emphasis>-EDM) beads

In this study, a new affinity high-performance liquid chromatography (HPLC) stationary phase suitable for protein separation was synthesized. In the first stage of the synthesis, uniform porous poly(2-hydroxyethyl methacrylate-co-ethylene dimethacrylate), poly(HEMA-co-EDM), beads 6.2 μm in size were obtained. Homogeneous distribution of hydroxyl groups in the bead interior was confirmed by confocal laser scanning microscopy. The plain poly(HEMA-co-EDM) particles gave very low non-specific protein adsorption with albumin. The selected dye ligand Cibacron blue F3G-A (CB F3G-A) was covalently linked onto the beads via hydroxyl groups. In the batch experiments, albumin adsorption up to 60 mg BSA/g particles was obtained with the CB F3G-A carrying poly(HEMA-co-EDM) beads. The affinity-HPLC of selected proteins (albumin and lysozyme) was investigated in a 25 mm×4.0-mm inner diameter column packed with CB F3G-A carrying beads and both proteins were successfully resolved. By a single injection, 200 μg of protein was loaded and quantitatively eluted from the column. The protein recovery increased with increasing flow rate and salt concentration of the elution buffer and decreased with the increasing protein feed concentration. During the albumin elution, theoretical plate numbers up to 30,000 plates/m were achieved by increasing the salt concentration.     

Decomposition of Triethylamine Over Acid Catalysts

The effect of hydrochloric acid, boric acid, and silica content in alumina on its catalytic activity towards the decomposition of triethylamine was investigated at 310°, 320°, and 330°. The study was carried out in a flow system and the reaction product was analyzed chromotographically. Ethylene formation is a zero order reaction independent of the partial pressure of triethylamine. Treating γ-alumina with hydrochloric acid increases its catalytic activity towards ethylene formation whereas silica-alumina is less active than γ-alumina. Boric acid-treated alumina has the same activity of γ-alumina. Formation of ethylene from preadsorbed triethylamine was studied. The similarity between reactions of aliphatic alcohols and amines over acid catalysts is concluded.     

Ru-catalyzed synthesis of substituted phthalides through C–H bond activation and functionalization

Synthesis of substituted phthalides through a ruthenium-catalyzed reaction of phthalic anhydrides with acrylates is described. The reaction proceeds via CH bond activation and leads to the formation of vinylated phthalides through a successive double vinylation accompanied by decarboxylation and annulation reactions.     

Catalytic Method for Synthesis of Aspirin by a Green,Efficient and Recyclable Solid Acid Catalyst (Preyssler's Anion) at Room Temperature

Synthesis of aspirin at room temperature via O‐acetylation of salicylic acid in the presence of Preyssler type heteropolyacids has been investigated in order to contribute toward clean technology, which is the most important need of the society. All of the catalysts are recyclable and reusable.     

Influence of hydrophobe content on the solution rheology of hydrophobically modified terpolymer of SO2, N,N-diallyl-N-carboethoxymethylammonium chloride

Rheological properties of hydrophobically modified copolymer of SO₂, N,N-diallyl-N-carboethoxymethylammonium chloride and the hydrophobic monomer N,N-diallyl-N-octadecylammonium chloride were studied. The influence of hydrophobe content (HP) and polymer concentration was investigated. Polymers with HP content in the range 1.5-5% were examined and the concentration was varied in the range 2-5 wt%. Both dynamic and steady-shear experiments were performed in ARES rheometer. Copolymers were observed to exhibit typical viscoelastic behavior even with low HP content. Both the dynamic viscosity, η′ and storage modulus, G′, increase with the increase of both the polymer concentration and the HP content of the system. The viscosity of the high HP content polymer showed a strong shear dependency, while G′ was a weak function of frequency and gel-like behavior was observed. The zero-shear viscosity, η₀, showed a strong concentration dependency (η₀ ∼ ?^α; 1.1 < α < 5.9). The concentration dependency of η₀ suggests that intermolecular association is dominant in the high HP content polymer. Control of the HP content and polymer concentration of this class of polymers can lead to a wide range of interesting rheological properties.     

Confirmation of eprinomectin, moxidectin, abamectin, doramectin, and ivermectin in beef liver by liquid chromatography/positive ion atmospheric pressure chemical ionization mass spectrometry

A liquid chromatographic (LC) multiresidue screening procedure was developed for determination of eprinomectin, moxidectin, abamectin, doramectin, and ivermectin in beef liver at 0, 25, 50, and 100 ppb levels. A procedure using low resolution LC/atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) was developed with further purification steps added to the quantitative LC method to confirm residues. Acetonitrile extracts of liver, prior to derivatization for LC analysis, were further purified by using a C8 solid-phase extraction cartridge and an alumina-B cartridge. The purified extract was analyzed by injection into an LC/positive ion APCI MS. Identity of the compound was confirmed by comparison of its retention time and relative intensity data with those of a standard or recovery from a fortified control liver sample. Anthelmintic drugs in acetonitrile extracts of liver containing eprinomectin, moxidectin, abamectin, doramectin, and ivermectin at 25 ppb, the lowest level of fortification used in the LC determinative method, were successfully confirmed.     

Synthesis of trimethyl (2S,3R)- and (2R,3R)-[2-H1]-homocitrates and the corresponding dimethyl ester lactones—towards elucidating the stereochemistry of the reaction catalysed by homocitrate synthase and by the Nif-V protein

Trimethyl (2S,3R)- and (2R,3R)-[2-²H₁]-homocitrates, 10b and 10c respectively, and dimethyl (2S,3R)- and (2R,3R)-[2-²H₁]-homocitric lactones, 11b and 11c respectively, have been synthesised from shikimic acid and [2-²H]-shikimic acid by a route which defines the stereochemistry of the two chiral centres in each compound. The NMR spectra of these products will enable the stereochemistry of the biological reaction catalysed by homocitrate synthase and by the protein from the nifV gene to be elucidated.     

Mild and Efficient Deprotection of 1,3‐Dithianes with N,N′‐ Diiodo‐N,N′‐1,2‐Ethanediyl‐Bis(p‐Toluenesulphonamide)

Aliphatic and aromatic 1,3‐dithiane are oxidized to the corresponding carbonyl compounds in good yields under mild conditions by N,N′‐diiodo‐N,N′‐1,2‐ethanediyl‐bis(p‐toluenesulphonamide) [NIBTS] and silver nitrate.