Solid phase extraction of lead by Chelest Fiber Iry (aminopolycarboxylic acid-type cellulose)

Aminopolycarboxylic acid-type cellulose (Chelest Fiber Iry) has been studied for its sorption efficiencies with respect to lead from acidic solution. The influence pH and other properties related to sorption kinetic, isotherm, maximum capacity, stability and the mechanism of the sorption were discussed.Lead was quantitatively retained on the proposed adsorbent in the pH range of 2.5-5.5 (studied pH range 1.5-5.5). The maximum sorption capacity was found to be 0.86±0.06 mmol/g adsorbent. The decline in the efficiency of the adsorbent was not observed for repeated adsorption-desorption cycles. It was found that the preconcentration factor of 200 can be achieved. The limit of determination was found to be about 1 μg Pb/2 l. The method was applied to the determination of lead in water samples.     

Cobalt-carbene complex with single-bond character: intermediate for the cobalt complex-catalyzed cyclopropanation

It is generally considered that metal-carbene carbon bonds in carbene complexes for cyclopropanation should be double-bonded; however, the theoretical and FT-IR analyses revealed that the cobalt-carbene carbon bond of the 3-oxobutylideneaminato or the salen-cobalt-carbene complexes was characterized as a single bond.     

Aurisides A and B, Cytotoxic Macrolide Glycosides from the Japanese Sea Hare Dolabella auricularia

Bioassay-guided fractionation of the cytotoxic constituents of the Japanese sea hare Dolabella auricularia led to the isolation of two novel cytotoxic compounds, aurisides A (1) and B (2). Their gross structures were established by spectroscopic analysis including the 2D NMR technique. On the basis of the NOESY spectral analysis and the degradation experiments, their absolute stereostructures were determined to be 14-membered macrolide glycosides that contain a bromine-substituted conjugated diene structure, a cyclic hemiacetal moiety, and a 2,4-di-O-methyl-L-rhamnopyranoside part. Aurisides A (1) and B (2) show cytotoxicity against HeLa S(3) cells with IC(50) values of 0.17 and 1.2 &mgr;g/mL, respectively.     

Preparation of sterically protected 3,4-bis[(2,4,6-tri-tert-butylphenyl)phosphinidene]cyclobutene derivatives having ring-fused structures

[reaction: see text] Sterically protected 3,4-diphosphinidenecyclobutenes, having ring-fused structures, were prepared. Structures of 8,9-bis[(2,4,6-tri-tert-butylphenyl)phosphinidene]bicyclo[5.2.0]non-1(7)-ene and its dichloropalladium(II) complex were analyzed by X-ray crystallography. A geometrical change induced by the complex formation was exhibited by X-ray crystallographic analysis. The geometrical change in solution was also suggested by (1)H NMR spectroscopy in CDCl(3).     

Thermally induced structural transformation in a hydrogen-bonded supramolecular single-crystal

The thermally induced structural transformation of a hydrogen-bonded crystal formed from an amphoteric molecule of 6-[2-methoxy-4-(pyridylazo)phenoxy]hexanoic acid MeO was studied using differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction measurement (XRD). Crystal form of the hydrogen-bonded crystal was measured by single crystal four circle diffractometer (Mo-K_α radiation). As a result, the crystal of MeO was stabilized by many C–H⋅⋅⋅O hydrogen bonds, and the C–H⋅⋅⋅O hydrogen bonds were broken by thermal energy reversibly. After transformation the supramolecular architecture was composed of supramolecular polymer including free-rotation pentamethylene main chains.     

Geometry for self-assembling of spherical hydrocarbon cages with methane thiolates on au(111)

An organodisulfide with a pair of adamantane moieties was synthesized, and its self-assembled monolayer (SAM) was formed on Au(111). The adamantane moieties are almost spherical and much bulkier than alkyl chains. The structure was characterized by scanning tunneling microscopy. Two-dimensional crystals of the SAM were found to be four orientationally different hexagonals with almost the same lattice constant with 4 radical 3a/3 and 7a/3 (a = 0.2884 nm, the Au lattice constant). The structure is assigned to four of the high-order commensurate adlayers. The present study of geometry and energetics for self-assembling of such an organosulfur compound with spherical cages provides a new insight into the probable SAM structure of various thiolate derivatives on Au(111).     

Synthesis of optically active β-alkyl aspartate via [3,3] sigmatropic rearrangement of α-acyloxytrialkylsilane

The synthesis of four types of optically active β-carbon-substituted analogs of threo-β-hydroxy aspartate (THA) and a β-carbon-substituted analog of threo-β-benzyloxy aspartate (TBOA), which are potent blockers of excitatory amino acid transporters in the mammalian central nervous system, via the chirality-transferring ester-enolate Claisen rearrangement of α-acyloxytrialkylsilane is described.