Frequency dependence of ionic conductivity and dielectric relaxation studies in Na3H(SO4)2 single crystal

Electrical impedance measurements of Na₃H(SO₄)₂ were performed as a function of both temperature and frequency. The electrical conductivity and dielectric relaxation have been evaluated. The temperature dependence of electrical conductivity reveals that the sample crystals transformed to the fast ionic state in the high temperature phase. The dynamical disordering of hydrogen and sodium atoms and the orientation of SO₄ tetrahedra results in fast ionic conductivity. In addition to the proton conduction, the possibility of a Na⁺ contribution to the conductivity in the high temperature phase is proposed. The frequency dependence of AC conductivity is proportional to ω^s. The value of the exponent, s, lies between 0.85 and 0.46 in the room temperature phase, whereas it remains almost constant, 0.6, in the high-temperature phase. The dielectric dispersion is examined using the modulus formalism. An Arrhenius-type behavior is observed when the crystal undergoes the structural phase transition.     

Column chromatographic preconcentration of palladium with dimethyl glyoxime and acenaphthenequinone dioxime on naphthalene

A solid material consisting of dimethyl glyoxime (DMG), acenaphthenequinone dioxime (ANDO) or DMG-ANDO on naphthalene provides a very convenient, rapid and economical method for the preconcentration of palladium in synthetic samples. Pd-DMG, Pd-ANDO and Pd-DMG-ANDO are quantitatively retained on naphthalene in the column in the pH ranges 2.2–4.4, 1.8–5.6 and 1.7–6.8, respectively. The solid mixture consisting of the metal complex together with naphthalene is stripped from the column with 5 ml of dimethylformamide (DMF)-n-butylamine and the absorbance is measured at 247.6 nm with an atomic absorption spectrometer. Calibration graphs are linear over the palladium concentration range 5–25 μg per 5 ml of the final solution for all the three complexes. Ten replicate determinations of a sample solution containing 10 μg of palladium gave mean absorbances of 0.180, 0.225 and 0.230 with relative standard deviations of 1.8, 1.7 and 1.6% using the reagents DMg, ANDO and DMG-ANDO, respectively. The sensitivity of the method is better than the direct atomic absorption spectrometric determination of palladium. It is highest in case of the mixed ligands, i.e., DMG-ANDO (0.038 μg ml^?1 for 1% absorption). The method can be applied to the trace determination of palladium in complex materials.     

Structure elucidation of AK-toxins,host-specific phytotoxic metabolites produced by alternaria kikuchiana tanaka

The structures of two host-specific phytotoxic metabolites, AK-toxin I and II, isolated from culture broth of Alternaria kikuchiana Tanaka (the fungus causing black spot disease of Japanese pear) were determined to be the ester consisting of N-acetyl-β-methyl-phenylalanine and 9,10-epoxy-8-hydroxy-9-methyl-2E, 4Z, 6E-decatrienoic acid ($\text{1}$) and its β-demethyl derivative ($\text{2}$).     

Development of fast disintegrating compressed tablets using amino acid as disintegration accelerator: evaluation of wetting and disintegration of tablet on the basis of surface free energy

A fast disintegrating compressed tablet was formulated using amino acids, such as L-lysine HCl, L-alanine, glycine and L-tyrosine as disintegration accelerator. The tablets having the hardness of about 4 kgf were prepared and the effect of amino acids on the wetting time and disintegration time in the oral cavity of tablets was examined on the basis of surface free energy of amino acids. The wetting time of the tablets increased in the order of L-lysine HCl, L-alanine, glycine and L-tyrosine, whereas the disintegration time in the oral cavity of the tablets increased in the order of L-alanine, glycine, L-lysine HCl and L-tyrosine. These behaviors were well analyzed by the introduction of surface free energy. When the polar component of amino acid was large value or the dispersion component was small value, faster wetting of tablet was observed. When the dispersion component of amino acid was large value or the dispersion component was small value, faster disintegration of tablet was observed, expect of L-tyrosine tablet. The fast disintegration of tablets was explained by the theory presented by Matsumaru.     

Mamanine and pohakuline,two unprecedented quinolizidine alkaloids from sophorachrysophylla

From the bark of the endemic Hawaiian tree Sophora chrysophylla Seem. we have isolated two unprecedented quainolizidine alkaloids, mamanine (4) and pohakuline (5). Both bases are 1-hydroxymethylenequinolizidines which are linked at C-3 to α-pyridone or α-piperidone moieties. The alkaloids may be intermediates in a heretofore unknown biogenetic pathway of Sophora alkaloids.     

Chemical studies on the anobiidae: Sex pheromone of the drugstore beetle, stegobium paniceum (L.) (coleoptera)

Chemical an spectroscopic evidence is presented to show that 2,3-dihydro-2,3,5-trimethyl-6-(1-methyl-2-oxobutyl)-4H-pyran-4-one (10) is the sex pheromone produced by the female drugstore beetle, Stegobium paniceum L.     

Synthesis of fluorine‐containing star‐shaped poly(vinyl ether)s via arm‐linking reactions in living cationic polymerization

Various types of fluorine‐containing star‐shaped poly(vinyl ether)s were successfully synthesized by crosslinking reactions of living polymers based on living cationic polymerization. Star polymers with fluorinated arm chains were prepared by the reaction between a divinyl ether and living poly(vinyl ether)s with fluorine groups (C₄F₉, C₆F₁₃, and C₈F₁₇) at the side chain using cationogen/Et_1.5AlCl_1.5 in a fluorinated solvent (dichloropentafluoropropanes), giving star‐shaped fluorinated polymers in high yields with a relatively narrow molecular weight distribution. The concentration of living polymers for the crosslinking reaction and the molar feed ratio of a bifunctional vinyl ether to living polymers affected the yield and molecular weight of the star polymers. Star polymers with block arms were prepared by a linking reaction of living block copolymers of a fluorinated segment and a nonfluorinated segment. Heteroarm star‐shaped polymers containing two‐ or three‐arm species were synthesized using a mixture of different living polymer species for the reaction with a bifunctional vinyl ether. The obtained polymers underwent temperature‐induced solubility transitions in various organic solvents, and their concentrated solutions underwent sol–gel transitions, based on the solubility transition of a thermoresponsive fluorinated segment. Furthermore, a slight amount of fluorine groups were shown to be effective for physical gelation when those were located at the arm ends of a star polymer. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012     

Synthesis and Antibacterial Activity of 3‐(Substituted arylmethyl)‐4‐acylaminomethyloxazolidin‐2‐ones and Derivatization to Symmetrical Twin‐Drug Type Molecules

In connection with our studies on antibacterial active compounds in the class of new oxazolidinones against Gram‐positive (Staphylococcus aureus) and Gram‐negative (Escherichia coli) strains, some molecular modifications were attempted. In this study, molecular modifications of 4‐aminomethyloxazolidin‐2‐ones ( 3a ) to the corresponding 4‐acylaminomethyloxazolidin‐2‐one derivatives ( 3c–d ) and preparations of the represented twin‐drug type molecules ( 10–14 ) were investigated. Some additional 4‐dialkylaminomethyloxazolidin‐2‐ones ( 2 ) were also synthesized. The synthesized compounds were evaluated for antibacterial activity with Gram‐positive (S. aureus) and Gram‐negative (E. coli) strains.     

Isolation and structure elucidation of genuine oat phytoalexin,avenalumin I

The major phytoalexin from oat leaves has been identified as 2-[2-(4-hydroxyphenyDethenyl] -6-hydroxy-4H-3,1-benzoxazin-4-one ($\text{A}$).