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161.
Jinno K Sawada H Catabay AP Watanabe H Sabli NB Pesek JJ Matyska MT 《Journal of chromatography. A》2000,887(1-2):479-487
Packed column capillary electrochromatography (CEC), open-tubular CEC and microcolum liquid chromatography (LC) using a cholesteryl silica bonded phase have been studied to compare the retention behavior for benzodiazepines. It has been found that packed column CEC gives better resolution, faster analysis time than microcolumn LC for benzodiazepines maintaining similar selectivity except for some solutes which are charged species under the separation conditions. However, open-tubular CEC gave different selectivities to a larger extent for charged benzodiazepines from that which should be produced by the chromatographic properties of the cholesteryl silica phase. Charged species migration times are mainly influenced by electrophoretic mobility rather than the chromatographic interactions. 相似文献
162.
163.
A reaction of 5-cyano-1,3-dimethyluracil (1, R = CN) with acetone in base afforded 1,3,7-trimethylpyrido-[2,3-d]pyrimidine-2,4(1H,3H)dione ( 9a ) in a moderate yield. From a reaction mixture of 1 (R = CN) with butanone, 1,3,6,7-tetramethyl- and 7-ethyl-1,3-dimethylpyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione ( 9b and 9c , respectively) were isolated in low yields. When ethyl cyanoacetate or malononitrile was used in place of the ketone in the above reaction, 7-amino-6-ethoxycarbonyl- and 7-amino-6-cyano-1,3-dimethylpyrido[2,3-d]-pyrimidine-2,4(1H,3H)-dione ( 14a and 14b , respectively) were obtained in quantitative yields. A plausible mechanism for the formation of bicyclic compounds is discussed. 相似文献
164.
Watanabe M Ikagawa A Wang H Murata K Ikariya T 《Journal of the American Chemical Society》2004,126(36):11148-11149
Well-defined chiral Ru amido complexes promoted asymmetric Michael addition of 1,3-dicarbonyl compounds including malonates, beta-keto esters, and 1,3-diketones to nitroalkenes to give the corresponding adducts with excellent ees and in excellent yields. 相似文献
165.
Redoxable nanosheet crystallites of MnO2 derived via delamination of a layered manganese oxide 总被引:2,自引:0,他引:2
This paper reports on the swelling and exfoliation behavior of a layered protonic manganese oxide, H(0.13)MnO(2).0.7H(2)O, in a solution of tetrabutylammonium (TBA) hydroxide and the formation and characterizations of unilamellar two-dimensional crystallites of MnO(2). At low doses of TBA ions, layered manganese oxide was observed to undergo normal intercalation, yielding a TBA intercalated phase with a gallery height of 1.25 nm. With a large excess of TBA ions, osmotic swelling occurred, giving rise to a very large intersheet separation of 3.5-7 nm. In an intermediate TBA concentration range, the sample exhibited a broad X-ray diffraction profile with superimposed diffraction features due to intercalation and osmotic swelling. The component responsible for the broad profile was isolated by centrifuging the mixture twice at different speeds, and the recovered colloid was identified as a pile of MnO(2) nanosheets, corresponding to the individual host layer of the precursor layered manganese oxide. Observations by transmission electron microscopy and atomic force microscopy revealed high two-dimensional anisotropy with a lateral dimension of submicrometers and a thickness of approximately 0.8 nm. The nanosheet exhibited broad optical absorption with a peak at 374 nm (epsilon = 1.13 x 10(4) mol(-1) dm(3) cm(-1)). The restacking process of the colloidal MnO(2) nanosheets was followed by aging the colloid at a relative humidity of 95%. The broad diffraction pattern due to the exfoliated sheets weakened with time and eventually resolved into two sharp distinct profiles attributable to a TBA intercalation compound with an intersheet spacing of 1.72 nm and an osmotically swollen hydrate with >10 nm at a very early stage. As drying progressed, the former phase became more abundant without a change in interlayer distance, while the degree of swelling of the latter phase gradually decreased to 2.7 nm that remained unchanged on further aging. Subsequent drying at a lower humidity collapsed the 2.7 nm phase. The resulting single 1.72 nm phase was dehydrated by heating at 150 degrees C to produce a phase with a contracted interlayer spacing of 1.3 nm. 相似文献
166.
T. Fujii H. Yamana K. Takamiya M. Watanabe H. Moriyama 《Journal of Radioanalytical and Nuclear Chemistry》2002,253(2):199-204
Adsorption behavior of fission products in nitric acid solution on various alloys and metals was studied by using a multitracer produced by neutron irradiation of UO2. The adsorption behavior of the fission products 99Mo, 131I, 132Te, 140La, and 143Ce, and 239Np was simultaneously studied. Some chemical decontamination tests were also examined. Clear adsorption of 99Mo, 131I, and 132Te was observed, whereas adsorption of 140La, 143Ce, and 239Np was not. The adsorption characteristics were discussed by considering anion-exchange reaction and surface complexation. 相似文献
167.
Kazuhiro Endo Hideo Ihara Kazuhiro Watanabe Shun-Ichi Gonda 《Journal of solid state chemistry》1981,39(2):215-218
Transition-metal trisulfides, TiS3, NbS3, and TaS3, with a quasi-one-dimensional structure are investigated by X-ray photoelectron spectroscopic (XPS) measurements to obtain information on the valence band structures. The band structures at the Fermi level of these compounds correspond well to their transport properties. A shoulder is observed at the top of the valence band in NbS3 and TaS3, suggesting that this band is made up of the metal dz2 electrons. The dz2 band is occupied in NbS3 and TaS2 and empty in TiS3. The characteristic features at the top of the valence band in NbS3 imply the occurrence of dz2 band separation, which leads to a semiconducting nature. 相似文献
168.
Wakisaka M Ohkanda T Yoneyama T Uchida H Watanabe M 《Chemical communications (Cambridge, England)》2005,(21):2710-2712
We have obtained the first in situ STM atomic images of a CO adlayer on a Pt(100)-(1 x 1) electrode in 0.1 M HClO(4) solution, exhibiting a phase transition from c(6 x 2)-10CO to c(4 x 2)-6CO at E > 0.3 V vs. RHE. 相似文献
169.
The Lewis acid-mediated reactions of allene-ene compounds, derived from 3-methylcitronellal or dimethyl malonate, were carried out using various Lewis acids such as ethylaluminum dichloride, diethylaluminum chloride, titanium chloride, zinc chloride etherate, or boron trifluoride etherate, affording unexpectedly intramolecular [2+2]cycloaddition products under some particular reaction conditions without any formation of intramolecular ene reaction products. 相似文献
170.
Self-organization of cationic polymer particles through hydrophobic interaction on polymer films in aqueous system and characteristic
properties of the resulting particle monolayers were investigated. Cationic polymer particles bearing quaternary ammonium
groups on their surfaces effectively self-organized on polymer films. With an increase of the particle surface charge density,
the surface coverage and average aggregate size (N
a) decreased. The surface coverage control was accomplished by tuning the ionic strength of the media. The wettability of polymer
films for water was imparted by the formation of particle monolayers on them. Annealing of the particle monolayers resulted
in the increase of the adhesive strength, while the wettability for water was lost. Further improvements of both wettability
and adhesive strength of particle monolayers were achieved by the immobilization of silica colloids on the particle monolayers.
This method would be effective for the hydrophilization of polymer films. 相似文献