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排序方式: 共有193条查询结果,搜索用时 15 毫秒
1.
Toshiaki Asakai Ryota Minegishi Norie Inaba Yutaka Ishimura Mariko Murayama Tatsuhiko Tanaka 《Analytical sciences》2006,22(3):461-463
The drying conditions for primary standards of volumetric analysis have a significant effect on the titration results due to changes in the purity, stability and homogeneity. Amidosulfuric acid, a strong acid used as a reference material for volumetric analysis in Japan, was dried in a vacuum desiccator or heated at different temperatures, and then measured by Karl-Fischer titration, thermogravimetry/mass spectroscopy (TG-MS), ion chromatography and coulometric titration. The optimum drying conditions were at 50 degrees C for 24 h with crushing. 相似文献
2.
Keisuke Kato Chie Matsuba Hiroyuki Takayama Tomoyuki Mochida Tat'yana A. Peganova Oleg V. Gusev 《Tetrahedron》2006,62(42):9988-9999
The oxidative cyclization-carbonylation of meso-2-alkyl-2-propargylcyclohexane-1,3-diols mediated by Pd(II) with chiral bisoxazoline (box ligand) afforded bicyclic-β-alkoxyacrylates. Based on a ligand screening, 2,2′-isopropylidenebis[(4S,5R)-4,5-di(2-naphthyl)-2-oxazoline] ligand has been developed. The products with a chiral quaternary carbon were obtained in 71-100% yields with 85-95% ee. 相似文献
3.
Peroxotungstate immobilized on ionic liquid-modified silica as a heterogeneous epoxidation catalyst with hydrogen peroxide 总被引:6,自引:0,他引:6
Yamaguchi K Yoshida C Uchida S Mizuno N 《Journal of the American Chemical Society》2005,127(2):530-531
Peroxotungstate immobilized on ionic liquid-modified SiO2 is capable of heterogeneously epoxidizing a wide range of olefins with the maintenance of the catalytic activity of homogeneous analogue. The epoxidation was immediately stopped by the removal of the catalyst, and no tungsten species could be found in the filtrate after the removal of the catalyst. These results can rule out any contribution to the observed catalysis from the tungsten species that leached into the reaction solution, and the observed catalysis is truly heterogeneous in nature. Furthermore, the catalyst was reusable without the loss of the catalytic performance. 相似文献
4.
Kamoda S Nomura C Kinoshita M Nishiura S Ishikawa R Kakehi K Kawasaki N Hayakawa T 《Journal of chromatography. A》2004,1050(2):211-216
Carbohydrate chains in glycoprotein pharmaceuticals have important roles for the expression of their biological activities. Therefore, development of an assessment method for the carbohydrate chains is an important parameter for quality control of glycoprotein pharmaceuticals such as newly developed therapeutic antibodies. In this report, we applied capillary electrophoresis with laser-induced fluorescence detection to the analysis of carbohydrate chains after releasing with glycoamidase followed by derivatization with 3-aminobenzoic acid. We found that four major oligosaccharides present in antibody pharmaceuticals were successfully separated with good resolution. The present method showed good precision in both migration times and relative peak areas, and gave comparable accuracy with that using a derivatization method with 8-aminopyrene-1,3,6-trisulfonate. 相似文献
5.
Iida T Satoh H Maeda K Yamamoto Y Asakawa K Sawada N Wada T Kadowaki C Itoh T Mase T Weissman SA Tschaen D Krska S Volante RP 《The Journal of organic chemistry》2005,70(23):9222-9229
[Reaction: see text]. The synthesis of neuropeptide Y antagonist 1, currently under clinical investigation for the treatment of obesity, is described. The convergent synthesis from trans-spirolactone carboxylic acid intermediate 2a and aminopyrazole 3 is predicated on a stereoselective route to the former. The coupling reaction of ethyl 4-oxocyclohexanecarboxylate (10a) with lithiated isonicotinamide 11 was investigated in detail, but even optimized conditions only provided a 45:55 ratio of trans:cis isomers (12a:12b). While selective crystallization schemes were developed to isolate the thermodynamically less stable trans isomer 2a, improved stereocontrol was subsequentially achieved by the application of ketene chemistry. The ketene formation and quench was investigated under a variety of conditions aimed at maximizing the trans:cis ratio. Reacting a mixture of carboxylic acids 2a and 2b with POCl3 in THF, followed by concomitant addition of tert-butyl alcohol in the presence of TMEDA at 35 degrees C provided a 4:1 ratio of trans:cis tert-butyl esters (18a:18b) via in situ ketene formation. Ester hydrolysis, followed by selective crystallization of undesired 2b as the HCl salt, led to isolation of 2a in 47% overall yield. Aminopyrazole intermediate 3 was synthesized via the condensation reaction of 2-fluorophenylhydrazine hydrochloride (4a) with acrylonitrile derivative 5 in 65-70% yield. Coupling of advanced intermediates 2a and 3b via activation with thionyl chloride gave a 92% yield of 1. 相似文献
6.
Shinya Hamasaki Chie Sawauchi Masami Kamigaito Mitsuo Sawamoto 《Journal of polymer science. Part A, Polymer chemistry》2002,40(4):617-623
A fast living radical polymerization of methyl methacrylate (MMA) proceeded with the (MMA)2? Cl/Ru(Ind)Cl(PPh3)2 initiating system in the presence of n‐Bu2NH as an additive [where (MMA)2? Cl is dimethyl 2‐chloro‐2,4,4‐trimethyl glutarate]. The polymerization reached 94% conversion in 5 h to give polymers with controlled number‐average molecular weights (Mn's) in direct proportion to the monomer conversion and narrow molecular weight distributions [MWDs; weight‐average molecular weight/number‐average molecular weight (Mw/Mn) ≤ 1.2]. A poly(methyl methacrylate) with a high molecular weight (Mn ~ 105) and narrow MWD (Mw/Mn ≤ 1.2) was obtained with the system within 10 h. A similarly fast but slightly slower living radical polymerization was possible with n‐Bu3N, whereas n‐BuNH2 resulted in a very fast (93% conversion in 2.5 h) and uncontrolled polymerization. These added amines increased the catalytic activity through some interaction such as coordination to the ruthenium center. © 2002 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 40: 617–623, 2002; DOI 10.1002/pola.10148 相似文献
7.
S. Iwama N. Satomi M. Yamanaka S. Goto T. Ishimura H. Ito 《International Journal of Infrared and Millimeter Waves》1981,2(6):1199-1208
A high-power CW 27.972 m water vapor laser has been constructed in order to use as a light source of an interferometer for plasma diagnostics. The laser consists of 220 cm length and 2.0 cm small bore Pyrex glass discharge tube, semi-confocal resonator and Michelson coupler. From the measurement of cavity detuning curves, it is found that two waveguide modes, EH11 and EH21 oscillate. The increase of the output power is found to become more than seven times larger by adding He(50%)–H2(50%) mixed gas. Under the optimum condition, the maximum output power of 65 mW or the output power per unit cavity volume of 83 W/cm3 is obtained. 相似文献
8.
Yusuke Nakajima Takeshi Kawano Yusuke Taki Chie Kojima 《Research on Chemical Intermediates》2018,44(8):4745-4754
Collagen is a major component of the extracellular matrix, and collagen gels have been used as cell scaffolds. We previously prepared gold nanoparticle (AuNP)-embedded collagen gels (AuCol) to serve as cell scaffolds that were sensitive to visible light. We performed single cell detachment from this cell scaffold using a microscope equipped with a laser irradiation system. In the present study, we adjusted hydrogel thickness and AuNP concentration in AuCol, with a goal of improving cell detachment efficiency. Thin hydrogels became blackened after the laser irradiation, and thick hydrogels with high AuNP concentrations were not permeable to the laser light. We, therefore, prepared bilayer gels, composed of AuCol as the upper layer and intact collagen gel (Col) as the bottom layer. These bilayer gels allowed more effective cell detachment, because they were thick and optically transparent. Our results indicated that an AuCol/Col ratio of 2 enabled the highest cell detachment efficiency. Essentially, no cell damage was observed in our system, suggesting that this is a cell-friendly single cell separation system. 相似文献
9.
10.
Facile Synthesis of Dibenzopentalene Dianions and Their Application as New π‐Extended Ligands 下载免费PDF全文
Takuya Kuwabara Dr. Kazuya Ishimura Prof. Dr. Takahiro Sasamori Prof. Dr. Norihiro Tokitoh Prof. Dr. Masaichi Saito 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(25):7571-7575
Reduction of phenyl(silyl)ethynes with potassium followed by quenching with iodine gave dibenzopentalenes in moderate yields. The intermediates of the reactions, dipotassium dibenzopentalenides, were isolated. The first dibenzopentalene–transition‐metal complex was successfully synthesized. The ruthenium atoms are located above the six‐membered rings. However, X‐ray diffraction analysis and theoretical calculations revealed that the aromatic nature of the five‐membered rings was retained. The cyclic voltammetry of the Ru complex revealed two oxidation waves with relatively large separation. 相似文献