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Yamamoto Y Ishii J Nishiyama H Itoh K 《Journal of the American Chemical Society》2004,126(12):3712-3713
The Ru(II)-catalyzed [2+2+2] cyclotrimerization of alkynylboronates, propargyl alcohol, and terminal alkynes proceeded chemo- and regioselectively to give rise to arylboronates, which were subjected to Suzuki-Miyaura cross-coupling with aryliodides to afford highly substituted biaryls in 53-76% yields. 相似文献
14.
Summary The simultaneous stereospecific assay of four stereoisomers of diltiazem hydrochloride in bulk drug and aqueous solution was
developed using HPLC on a Chiralcel OF column. The four isomers were quantitated with good precision by the internal standard
method. The chiral inversion of (+)-cis-diltiazem hydrochloride in vitro, stability of its (2S, 3S) configuration in the solid
and aqueous states was examined by HPLC. Chiral inversion of (+)-cis-diltiazem hydrochloride was not observed in the solid
state, and its (2S, 3S) configuration was stable to heat, humidity and light. Chiral inversion of (+)-cis-diltiazem hydrochloride
(2S, 3S) was observed in aqueous solution under UV, but not in aqueous solution stored at 80°C for 5h nor under visible light
for 10 h. The (+)-cis-diltiazem hydrochloride (2S, 3S) epimerized to (+)-trans-diltiazem hydrochloride (2R, 3S) with a half-life
of 5h in aqueous solution under UV but the reverse chiral inversion of (+)-trans-diltiazem hydrochloride (2R, 3S) to (+)-cis-diltiazem
hydrochloride (2S, 3S) was not observed. 相似文献
15.
Y Kusumoto M Goto H Tajima K Nakata R Furukawa A Satoh K Kawahara N Ishii T Munehisa T Koji 《Radioisotopes》1984,33(10):686-690
To determine the diagnostic value of anti-HBc IgM in acute viral hepatitis or chronic liver disease B, Anti-HBc IgM was measured by a RIA and an ELISA in 32 patients with acute hepatitis (4 with type A, 15 with type B and 13 with type non A non B), 18 patients with chronic hepatitis and 19 patients with liver cirrhosis. In acute hepatitis B, anti-HBc IgM (both RIA and ELISA) was positive in 14(93%) of 15 patients and its cut-off index value was very high. However, anti-HBc IgM was always negative in one patient with typical course of type B. In 1 of 4 patients with acute hepatitis A and 2 of 13 with non A non B, anti-HBc IgM (RIA and/or ELISA) was positive. These 3 patients were positive for anti-HBs at the onset of disease, so we could not made the diagnosis of acute hepatitis B. Anti-HBc IgM was positive in 21(51%) of 37 patients with HBsAg-positive chronic liver disease by RIA and in 11 (30%) by ELISA, and its cut-off index value was relatively low. These results suggest that when adequate cut-off index value is established, anti-HBc analysis is useful for differentiating recent and current infections from remote infections. 相似文献
16.
Properties of fluorescence and the excitation spectra of fluorescein molecules adsorbed onto a calcinated (773 K) porous Vycor glass have been investigated as a function of the amount of adsorbed dye (the surface coverage, θ = 0.00051 and 0.0098). The fluorescence and fluorescence-excitation spectra of fluorescein adsorbed onto Vycor glass showed the spectrum only due to cation species at θ = 0.00051. On the other hand, the spectra observed at θ = 0.0098 suggested the presence of cation, anion, and dianion species on the surface of Vycor glass. These results indicated the existence of at least two different types of adsorption sites involving the Brønsted acid site on the surfaces of Vycor glass. 相似文献
17.
Fischer indolization of ethyl pyruvate 2-methoxyphenylhydrazone (1) with p-toluene-sulfonic acid in benzene in the presence of an enolizable dicarbonyl or an indolic compound gave either an indole product having an active methine group at C6 or a novel type of 3,6′-biindole compound. Structures of the products were established by NMR spectra and chemical evidence. 相似文献
18.
In the reaction of soybean lipoxygenase (EC 1.13.11.12) with polyunsaturated fatty acids such as linoleic, linolenic and arachidonic acids, some radical species were detected using the electron spin resonance (ESR) spin-trapping technique. The radical species derived from the three polyunsaturated fatty acids were not distinguishable because the ESR spectra of the spin adducts of nitrosobenzene with their three radical species showed no difference in their hyperfine splittings. To overcome this defect of the spin-trapping technique, these spin-adducts were separated by employing high-performance liquid chromatography (HPLC) combined with ESR spectroscopy. The spin adducts were eluted from a C18 reversed-phase column in the order linolenic acid, linoleic acid and arachidonic acid. The half-lives of the spin adducts separated by HPLC-ESR were determined as linoleic acid 600 min, linolenic acid 360 min and arachidonic acid 160 min. The use of an ultraviolet detector together with the HPLC-ESR technique resulted in a 500-fold increase in sensitivity in the detection of the radical species. 相似文献
19.
The intercalation of 4-phenylazoaniline (PAA) in supercritical carbon dioxide (SC-CO(2)) into montmorillonite (TMA-Mnt) pillared with tetramethylammonium ions at 313 K and 15 MPa was investigated. The adsorption rate and equilibrium PAA uptake were compared with those in n-hexane, CCl(4) and benzene solutions at 313 K. The XRD and N(2) adsorption/desorption analyses showed that TMA-Mnt after adsorption of PAA in SC-CO(2) had the same pore structure as after adsorption of PAA in normal solvents. SC-CO(2) was found to be a good medium for PAA adsorption owing to its having a relatively high adsorption rate and the highest adsorptivity at the same PAA concentration. The properties of PAA adsorption on TMA-Mnt could be well elucidated by the difference in solubility parameters between liquid and solid phases. 相似文献
20.
M. Ebihara Y. Oura T. Ishii M. Setoguchi H. Nakahara T. Ohtsuki 《Journal of Radioanalytical and Nuclear Chemistry》2000,244(3):491-496
Chondritic meteorite samples were analyzed nondestructively by photon activation analysis. Powdered samples weighing about 50 mg each were irradiated with photons (-rays) converted from electrons accelerated by a linear electron accelerator at 20 and 30 MeV. With 30-minute and 6-hour irradiations, 11 and 12 elements with duplication of 6 elements could be determined, respectively. Considering that several major elements including Mg, Si and Fe can be determined in addition to Ti, Rb, Sr, Y and Zr, which cannot or hardly be determined by instrumental neutron activation analysis (INAA) with rather high sensitivity, instrumental photon activation analysis is as effective as INAA. 相似文献