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1.
The molybdenum and tungsten dinitrogen-organonitrile complexes trans-[M(N2)(NCR)(dppe)2] (2, M=Mo; 4, M=W; R=Ph, C6H4Me-p, C6H4OMe-p, Me; dppe=Ph2PCH2CH2PPh2) underwent double protonation at the nitrile carbon atom with loss of N2 and a change in oxidation state to +4 on treatment with hydrochloric acid to afford the cationic imido complexes trans-[MCl(NCH2R)(dppe)2]+. The solid-state structure of trans-[WCl(NCH2CH3)(dppe)2][PF6]·CH2Cl2 was determined by single-crystal X-ray analysis. Protonation of complexes 2 by fluoroboric acid or hydrobromic acid also formed the similar imido complexes trans-[MoX(NCH2R)(dppe)2]+ (X=F, Br). In contrast, the dinitrogen complex trans-[Mo(N2)2(dppe)2] reacted with two equiv. of benzoylacetonitrile, a nitrile with acidic CH hydrogen atoms, to give the nitrido complex trans-[Mo(N)(NKCCHCOPh)(dppe)2] (12), which was accompanied by evolution of dinitrogen and the formation of 1-phenyl-2-propen-1-one in high yields. For complex 12, the zwitterionic structure, where the anionic enolate ligand PhC(O+)=CHCN coordinates to the cationic Mo(IV) center through its nitrogen atom, was confirmed by spectroscopic measurements and single-crystal X-ray analysis. A unique intermolecular aromatic C---HO hydrogen bonding was observed in that crystal structure. Complex 12 is considered to be formed via the cleavage of the CN triple bond of benzoylacetonitrile on the metal. A reaction mechanism is proposed, which includes the double protonation of the nitrile carbon atom of the ligating benzoylacetonitrile on a low-valent molybdenum center. 相似文献
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C Hamada N L Sato S Niimura A Kato N Fujisawa Y Maeda T Kumanishi H W Lee 《Jikken dobutsu》1986,35(1):1-9
An assay method for the infectivity of Hantaan virus, a causative agent of HFRS (hemorrhagic fever with renal syndrome), was developed by the use of IFA (immunofluorescent antibody technique). With the aid of this method, the growth characteristics of Hantaan virus, 76-118 strain, were followed in A549 cells. At a maximal MOI (multiplicity of infection) of 1.6 VAIU (viral antigen-inducing units) per cell, the conventionally available value, plateau level potencies of the viral antigen and virus infectivity were attained at eight and ten days postinfection, respectively, and most of the infective virus produced accumulated in the culture fluids of infected cells. When infections were defined with MOI values in terms of VAIU per cell, development of the viral antigen was highly consistent and followed a given pattern of kinetics. Based on these findings, a protocol for preparation of the viral antigen in IFA was presented, wherein spot culture and FBS treatment were emphasized as effective procedures to minimize non-specific staining. 相似文献
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Novel mono-O-acetylated GM3s, one containing 9-O-acetylN-glycolyl neuraminic acid and another containing 6-O-acetyl galactose, were isolated as a mixture from equine erythrocytes, and the structures were characterized by one- and two-dimensional proton nuclear magnetic resonance (NMR) and fast atom bombardment-mass spectrometry (FAB-MS). The position of theO-acetyl residue was identified by the downfield shift of the methylene protons at C-9 ofN-glycolyl neuraminic acid (9-O-Ac GM3) and C-6 of galactose (6-O-Ac GM3) in the NMR spectrum, in comparison to the respective non-acetylated counterparts. To confirm the presence of 6-O-Ac GM3, theO-acetylated GM3 mixture was desialylated withArthrobacter neuraminidase, giving 6-O-acetyl galactosyl glucosylceramide, the structure of which was estimated by NMR and FAB-MS, together with non-acetylated lactosylceramide with a ratio of 1:1.
Abbreviations: Ac, acetyl; Gc, glycolyl; NeuGc,N-Gc neuraminic acid; GM3 (Gc), GM3 containing NeuGc (II3NeuGc-LacCer); 4-O-Ac GM3 (Gc), GM3 containing 4-O-Ac NeuGc; 9-O-Ac GM3 (Gc), GM3 containing 9-O-Ac NeuGc; 6-O-Ac GM3 (Gc), GM3 containing 6-O-Ac Gal; 1D-NMR, one-dimensional nuclear magnetic resonance spectrometry; 2D-COSY, two-dimensional chemical shift-correlated spectrometry; FAB-MS, fast atom bombardment-mass spectrometry; GLC, gas-layer chromatography; GC-MS, gas chromatography-mass spectrometry; TLC, thin-layer chromatography; Ggl, ganglioside; Cer, ceramide; CMH, monohexosylceramide; LacCer, lactosylceramide; 6-O-Ac LacCer, LacCer containing 6-O-Ac Gal; Me2SO-d6,2H6-dimethylsufloxide; CMW, chloroform-methanol-water; Nomenclature and abbreviations of glycosphingolipids follow the system of Svennerholm (J Neurochem [1963]10: 613–23) and those recommended by the IUPAC-IUB Nomenclature Commission (Lipids [1977]12: 455–68). 相似文献
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Small angle neutron scattering (SANS) method was used to study lysozyme solutions, with particular interest in an understanding of the crystallization process at the initial stage. It is found that (1) in the unsaturated solution, the protein molecules aggregate with a continuous increase in size when NaCl concentration is increased, and (2) in the supersaturated solution, an irreversible change, superimposed on the former process, occurs when the supersaturation is realized. These facts indicate the usefulness of SANS in detecting changes of protein molecules in solution on the nanometer scale. The reliability of the SANS results are indicated by (1) comparing them with those of small angle X-ray scattering (SAXS), and (2) comparing the effect of D(2)O and H(2)O as solvent. Since the interparticle interaction is essential in the crystallization process and a simple Guinier plot analysis is not allowed, a more rigorous framework of analyzing data with interference function is developed, through which both average interparticle distance and particle size are estimated. 相似文献
8.
Takeshi Nishimura Setsuko Yamamoto Takaaki Yamamoto Munekiyo Kaneko Youichi Hara 《Prostaglandins & other lipid mediators》1996,51(2):149-159
The antithrombotic effect of topical application of the 3-oxamethano-prostaglandin (PG) I1 analog, SM-10902 in the microcirculation and in vitro antiplatelet functions of its active form SM-10906 were estimated in comparison with PGI2 and PGE1. In rat platelets, SM-10906 evoked accumulation of intracellular cyclic adenosine 3′,5′-monophosphate, and exhibited antiaggregatory and disaggregatory activities, which were all enhanced by the phosphodiesterase inhibitor theophylline. Additionally, SM-10906 was shown to inhibit platelet adhesion to collagen in human platelet-rich plasma. PGI2 and PGE1 also showed in vitro antiplatelet effects in the order of PGI2 > SM-10906 ≥ PGE1. SM-10902 exhibited a dose-dependent antithrombotic effect in the guinea pig mesenteric arteriole by a topical application, and this activity might be exerted by the antiplatelet functions of SM-10906. Although SM-10906, PGI2 and PGE1 also showed the antithrombotic effects, SM-10902 was the most potent. In conclusion, the present studies indicate that an external topical preparation of SM-10902 may be useful for the therapy of peripheral circulatory insufficiency. 相似文献
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Youichi Kawakita Masaki Seto Tomohiro Ohashi Toshiya Tamura Tadashi Yusa Hiroshi Miki Hidehisa Iwata Hidenori Kamiguchi Toshimasa Tanaka Satoshi Sogabe Yoshikazu Ohta Tomoyasu Ishikawa 《Bioorganic & medicinal chemistry》2013,21(8):2250-2261
A novel 7,6 fused bicyclic scaffold, pyrimido[4,5-b]azepine was designed to fit into the ATP binding site of the HER2/EGFR proteins. The synthesis of this scaffold was accomplished by an intramolecular Claisen-type condensation. As the results of optimization lead us to 4-anilino and 6-functional groups, we discovered 6-substituted amide derivative 19b, which has a 1-benzothiophen-4-yloxy group attached to the 4-anilino group. An X-ray co-crystal structure of 19b with EGFR demonstrated that the N-1 and N-3 nitrogens of the pyrimido[4,5-b]azepine scaffold make hydrogen-bonding interactions with the main chain NH of Met793 and the side chain of Thr854 via a water-mediated hydrogen bond network, respectively. In addition, the NH proton at the 9-position makes an additional hydrogen bond with the carbonyl group of Met793, as we expected. Compound 19b revealed potent HER2/EGFR kinase (IC50: 24/36 nM) and BT474 cell growth (GI50: 18 nM) inhibitory activities based on its pseudo-irreversible (PI) profile. 相似文献
10.
Youichi Tamai Hiroshi Shinmoto Masayoshi Takakuwa 《Bioscience, biotechnology, and biochemistry》2013,77(12):2713-2721
A thermo-labile antigen (TLA) on the yeast cell surface was isolated from a yeast cell autolyzate and purified to a homogeneous state by chromatography on an immunoadsorbent affinity column. The molecular weight of TLA was about 1.45 x 105 on SDS-polyacrylamide gel electrophoresis and about 1.5 x l05 on gel chromatography on Sephadex G-200. The TLA contained 74.5% protein and 25.5% sugar. It was characterized by high contents of glycine, glutamic acid, serine and aspartic acid. Half-cystine, methionine, histidine and arginine were not found. The sugar moiety was composed of galactose, mannose, N-acetylglucosamine and fucose. The antigenic determinant of TLA was distinct from that of cell wall mannan in the Ouchterlony immunodiffusion test. No precipitin line against anti-TLA serum was observed, when TLA was heated at 90°C for 10 min. Oxidation with periodate had little effect on antigenicity, but digestion with Pronase or treatment with protein denaturants resulted in loss of the antigenicity. These results suggest that the protein moiety plays an important role as the antigenic determinant of TLA. Moreover, the antiserum specific to TLA agglutinated fresh yeast cells, and the distribution of TLA was apparent on the yeast cell surface by immunofluorescence staining. These findings suggest that TLA molecules were exposed on the outer surface of the yeast cell wall. 相似文献