“Ghost peaks” of olmesartan medoxomil: Two solution degradation products of olmesartan medoxomil via oxidation mediated by metal ions

Two unknown solution degradants were found during the dissolution testing in 0.1-M HCl for olmesartan medoxomil (OLM) tablets. The structure of the degradants was identified and characterized by liquid chromatography–ultraviolet (LC–UV), liquid chromatography with tandem mass spectrometry (LC–MS/MS), and nuclear magnetic resonance (NMR) and demonstrated to be cyclization of tetrazole and benzene in the olmesartan (OL) and OLM structures. A series of studies including stress studies, simulation studies, and mechanism-based studies were performed to reveal the potential mechanisms that lead to the formation of the unknown degradants. The study results demonstrated that the degradation was catalyzed with radicals that originated from the metal ions leached from the inner surface of high-performance liquid chromatography (HPLC) glass vials with dissolved oxygen under acidic condition. Prerinsing the glass vials with acidic solution dissolved with EDTA can effectively avoid the generation of such oxidative impurities. The present work provides new insights into the understanding of degradation pathways of OLM, which might support the development of OLM tablets.     

Cationic para‐phenyl‐substituted α‐diimine nickel catalyzed ethylene and 4‐methyl‐1‐pentene (co)polymerizations via living/controlled chain‐walking

Upon activation with diethylaluminium chloride (Et₂AlCl), a series of phenyl‐substituted α‐diimine nickel precatalysts conducted 4‐methyl‐1‐pentene (4MP) and ethylene (E) (co)polymerizations via controlled chain‐walking to generate branched amorphous polymers with high molecular weight and narrow molecular weight distribution (M_w/M_n < 1.6). The obtained poly(4MP)s were amorphous elastomers with glass transition temperature (T_g) of ?10 ~ ?24 °C, which are higher than that of E‐4MP copolymer ( ? 63.0 °C). At room temperature (25 °C), 4MP polymerization proceeds in a living manner. The microstructures of the produced poly(4MP)s indicated the 2,1‐ and 1,2‐insertion followed by chain‐walking, the latter being predominant. The NMR analyses of the polymers showed that the obtained poly(4MP) possessed methyl, isobutyl, 2,4‐dimethylpentyl and 2‐methylhexyl groups, while the isobutyl and 2,4‐dimethylalkyl branches derived from 4MP were observed in the E‐4MP copolymer. The branch structures and the insertion‐type of monomer were depended on the polymerization temperature, and the content of methyl branch increased with an increase in the polymerization temperature.     

Precision Chain‐Walking Polymerization of trans‐4‐Octene Catalyzed by α‐Diimine Nickel(II) Catalysts Bearing ortho‐sec‐Phenethyl Groups

α‐Diimine nickel complexes bearing bulky ortho‐sec‐phenethyl groups (bis{[N,N′‐(4‐methyl‐2,6‐di‐sec‐phenethylphenyl)imino]‐1,2‐dimethylethane}dibromonickel ( 1 ), bis{[N,N′‐(4,6‐dimethyl‐2‐sec‐phenethylphenyl)imino]‐1,2‐dimethylethane}dibromonickel ( 2 ), bis{[N,N′‐(4‐methyl‐2‐sec‐phenethylphenyl)imino]‐1,2‐dimethylethane}dibromonickel ( 3 )) and {bis[N,N′‐(2,4,6‐trimethylphenyl)imino]‐1,2‐dimethylethane}dibromidonickel ( 4 ) are used as a precatalyst for the polymerization of trans‐4‐octene upon activation with modified methylaluminoxane. These catalysts conduct chain‐walking polymerization of trans‐4‐octene to give polymers possessing propyl and butyl branches with high molecular weight and narrow molecular weight distribution. The branching structure depends on the nickel complex as well as the polymerization temperature, and the ratio of propyl branch was increased with increasing the bulkiness of the ligand and decreasing the polymerization temperature. Consequently, the most bulky 1 among the complexes used is found to polymerize trans‐4‐octene with high 1,5‐regioselectivity at −20 °C to give poly(1‐propylpentan‐1,5‐diyl).

     

ON COMPACT COMPOSITION OPERATORS ON A CLASS OF HOLOMORPHIC FUNCTION SPACES OVER THE UNIT BALL IN C~n

In this paper, a general function space X(B n ) over the unit ball in C n with norm · X(Bn) is introduced. It contains all Hardy space, Bergman space, Besov space etc. The author gives a formulation of a compact composition operator on X(B n ), related to works of [8] and [10].     

Structures and properties of functional metal iodates

Metal iodates with a lone-pair containing I(V) that is in an asymmetric coordination geometry can form a diversity of unusual structures and many of them are promising new second homonic generation (SHG) materials. They exhibit wide transparency wavelength regions, large SHG coefficients and high optical-damage thresholds as well as moderately high thermal stability. In this paper, the structures and properties of the metal iodates are reviewed. The combination of d0 transition-metal cations with the iodate...     

Synthesis,X-Ray Structure and Characterization of a Triruthenium Cluster Complex Ru_3~Ⅲ(μ_3-O)(μ-CH_3COO)_6(py)_2Cl with Four Steps One-electron Redox Processes

Great attention is currently paid to the synthesis of polynuclear transition metal complexes as well as their photochemical, photophysical, and electrochemical properties. The design of multicomponent systems capable of performing useful light- and/or redox-induced function is of special interest1. The oxo-centered carboxylate-bridge trinuclear ruthenium clusters have been investigated extensively during recent decades because they have remarkable electron-transfer properties, intense visibl…     

Hydrothermal Synthesis and Characterization of a Novel Two-dimensional Framework Materials Constructed from Polyoxometalate and Coordination Groups: [H_2Mo_(5.5)V_(10.5)O_(40)(PO_4)][Cu(en)_2]_4·7H_2O

IntroductionPolyoxometalatesarewidelystudiedfortheirin terestingapplicationsincatalysis ,electronicconduc tivity ,magnetism ,nonlinearopticsandmedicine[1— 4 ] .Whilethemechanismofthesynthesisofpolyoxometalatesremainselusiveandisoftende scribedasself assembly ,thereseemstobeanincreas inguseofthecombinationofthehydrothermalmethodandthestructure directingtemplate .There searchwiththismethodhasdemonstratedthatanum beroftransitionmetaloxides ,typicallyreducedmolybdenumoxides ,mixedvalancevanadiumo…     

混杂配体金属簇合物的分子振动光谱与结构

由于原子簇化合物在催化，生物活性，功能材料等方面所呈现的重要性，使其成为无机和物理化学最重要的研究领域之一。文章中和谱学方法对一些具有混配体的过渡金属簇合物的结构及其两者之间的关系进行.     

Ab Initio and Density Functional Study on the First Hyperpolarizabilities of Squaric Acid Homologues

The first hyperpolarizabilities of four squaric acid homologues: squaric acid, 1,2-dithiosquaric acid,1,2-diselenosquaric acid and 1,2-ditellurosquaric acid have been calculated using ab initio and DFT methods. The effects of equilibrium geometries, basis set and electron correlation on the first hyperpolarizabilties of these molecules were investigated. The frequency dispersion effect and solvent effect, which are essential to get reliable outputs in comparison to the experimental results, have also been explored. On the basis of these investigations, it is worthy to point out that the heavy atom effect takes effect for these squaric acid homologues.