Dielectrically controlled resolution (DCR) of 3-aminopiperidine via diastereomeric salt formation with N-tosyl-(S)-phenylalanine

A useful key intermediate for the dipeptidyl peptidase-4 (DPP-4) inhibitor, 3-aminopiperidine 1, was successfully resolved with an enantiomerically pure resolving agent, N-tosyl-(S)-phenylalanine 2, to give both stereoisomers (R)-1 and (S)-1 as a less-soluble diastereomeric salt with (S)-2, via a dielectrically controlled resolution (DCR) phenomenon.     

Synthesis of ZrO<Subscript>2</Subscript> nanoparticles for liquid scintillators used in the detection of neutrinoless double beta decay

We synthesized liquid scintillators incorporating ZrO₂ nanoparticles for application in neutrinoless double beta decay experiments. ZrO₂ nanoparticles of less than 10 nm in size were synthesized with sub- and supercritical hydrothermal methods. The Zr concentrations in the liquid scintillators were determined to be up to 1.4 wt% with inductively coupled plasma analysis, and the liquid scintillators were transparent to scintillation. These results indicate that these methods are applicable for the preparation of liquid scintillators for neutrinoless double beta decay experiments.     

Epoxidation of Allylic Alcohols with Hydrogen Peroxide Catalyzed by [PMO12O40]3-[C5H5N+(CH2)15CH3]3

Applicatims a Mo- and W-based heteropoly acids (HPA) as a catalyst in the oxidation of olefins have extensively been investigated¹. However, a patent work is only attempted concerning the evoxidatim of olefins with H₂0₂ by HPA²⁾ since the oxirane ring is cleaved because of a strong acidity of HPA itself. Herein, an effective epoxidatim of some allylic alcohols with H₂0₂ by a new Mo-species (MPCP), which was prepared from 12-molybdatophosphoric acid (H₃PMo₁₂0₄₀) and cetylpyridinium chloride (C₅H₅N (CH₂), ₁₅CH₃- C1^-) under two-phase conditions using chloroform as an organic solvent, is described.     

NMR‐based analysis of the chemical composition of Japanese persimmon aqueous extracts

Japanese persimmon (Diospyros kaki L.) is recognized as an outstanding source of biologically active compounds relating to many health benefits. In the present study, NMR spectroscopy provided a comprehensive metabolic overview of Japanese persimmon juice. Detailed signal assignments of Japanese persimmon juice were carried out using various 2D NMR techniques incorporated with broadband water suppression enhanced through T₁ effects (BB‐WET) or WET sequences, and 26 components, including minor components, were identified. In addition, most components were quantitatively evaluated by the integration of signals using conventional ¹H NMR and BB‐WET NMR. This is the first detailed analysis combined with quantitative characterization of chemical components using NMR for Japanese persimmon. Copyright © 2015 John Wiley & Sons, Ltd.     

Structures and Reaction Mechanism of Novel Metal-Carbene Complexes Derived from Hypervalent Diazadiselenathiapentalenes

Abstract

Novel metal-carbene complexes (4) with a metallapentalene framework have been obtained from hypervalent diazadiselenathiapentalenes (3) by treating with Pt(PPh₃)₄, Pd(PPh₃)₄ and RhCl(PPh₃)₃. X-Ray investigations revealed that the central hypervalent sulfur atom in 3 was substituted by a metal atom to form M-Se bonds in the resultant metallapentalene framework.     

Deformation Electron-Density Distributions of Tetraazathiapentalenes with Hypervalent S-N Bonds

Abstract

The deformation electron-density distributions of 6a-thia-1,3,4,6-tetraazapentalene derivatives (I, II) and bis(phenylthio)dibenzothiophene (III) were investigated by the X-ray diffraction method. For I and II, a structure around the hypervalent S-N bonds is a trigonal bipyramid with equatorial sp² hybrid of S-C bond and lone-pair electrons and apical polarized S-N bonds. In 111 lone-pair electron densities are observed perpendicular to the thiophene ring and the C-S-C sulfide planes.     

Preparation of Ring and Chain Condensed Oligophosphates

Preparations of small-ring and short-chain condensed phosphates were made by dry and wet processes, respectively. The crystallization of tetra- hexa-, and octaphosphates from the phosphate solution was not easy, and metal salts of these oligophosphates were amorphous and unstable at normal temperature. Guanidine tetraphosphate and ammonium hexaphosphate were crystalline and stable at normal temperature.     

DNA sensor: A novel electrochemical gene detection method using carbon electrode immobilized DNA probes

Abstract

The authors have developed a novel, rapid, convenient, and specific gene detection method, named the ‘DNA sensor,’ using a graphite electrode loaded with DNA probes. Synthesized oligonucleotide (5-TGCAGTTCCGGTGGCTGATC-3′) complementary to oncogene v-myc was employed for a model probe. The oligonucleotide was chemically adsorbed on a basal plane pyrolytic graphite (BPPG) electrode. The sensor was able to be applied to a hybridization reaction (40°C) in a linearized pVM623 solution carrying the Pst I fragment of v-myc (1.5 kbp).

After the hybridization reaction, the sensor was immersed into an acridine orange solution (1 μM) and washed with a phosphate buffer (pH 7.0). Acridine orange intercalated between base pairs of the formed double stranded DNAs on the electrode. The anodic peak potential of acridine orange that interacted with the DNAs on the electrode was measured. The positive shift of the peak potential increased in proportional to the pVM623 concentration in the hybridization reaction. 10^?1 g/ml of pVM623 was able to be detected in the buffer solution using the sensor. This gene detection was completed within an hour.