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61.
The Beckmann fragmentation product, 3-methoxy-17-oxo-16,17-secoestra-1,3,5(10)-trien-16-nitrile (2) has been reduced by LAH giving the expected 3-methoxy-17-hydroxy-16,17-secoestra-1,3,5(10-trien-16-amine hydrochloride (3) and 3-methoxy-17-oxa-D-homoestra-1,3,5(10)-trien-16-ol (4), by a presumed neighbouring group participation of 17-OH group in the intermediary formed 16-imino derivative (A). The structure of 4 has been proved by an alternative synthetic route by reducing 3-methoxy-17-oxa-D-homoestra-1,3,5(10)-trien-16-one (7) with di-iso-butylaluminium hydride. 相似文献
62.
Perišić-Janjić Nada U. Ž. Jovanović Bratislav Janjić Natasa J. Rajković Olga S. Antonović Dušan G. 《平面色谱法杂志一现代薄层色谱法》2003,16(6):425-432
JPC – Journal of Planar Chromatography – Modern TLC - The chromatographic behavior of nine newly synthesized s-tri-azines has been studied by thin-layer chromatography on C18/UV254... 相似文献
63.
Jadranka Vuković Shiro Matsuoka Kazuhisa Yoshimura Vladimir Grdinić Renata Jurišić Grubešić 《Mikrochimica acta》2007,159(3-4):277-285
A simple, sensitive and rapid solid-phase spectrophotometric procedure was developed for the determination of traces of phenol
with 4-aminoantipyrine as a reagent (AAP-SPS), and the optimal experimental conditions were established. This method was performed by sorption and direct absorbance measurements
of the product phenol-AAP sorbed on the anion-exchanger Dowex 1-X4 (0.2 g) at 495 nm (absorption maximum) and 700 nm (non-absorption wavelength). The
sensitivity offered by the AAP-SPS procedure was higher by a factor of 40 compared with the respective conventional spectrophotometric method. Metrological
characteristics were established using a prevalidation strategy. The AAP-SPS procedure is characterized by a linear calibration function in the working range of 0.05–0.50 μmol, low standard deviation
of procedure (±0.012), low limit of determination (0.021 μmol), and favorable random (±0.85 to ±11.27%) and systematic deviations
(−4.55 to +11.50%). Moreover, the accuracy of the system investigated by the recovery test is acceptable (99–102%). Favorable
working and performance characteristics make the new SPS method ideal for phenol monitoring in pharmaceutical preparations
as well as other matrices. 相似文献
64.
The reduction of Ni2+ ions at mercury electrodes in acidic perchlorate solutions, at perchlorate concentrations below 0.2 M, is characterized by absence of kinetic control in the preceding step, and by a complex reaction mechanism following the electron transfer. This reaction sequence is known to involve intermetallic compound formation between Ni and Hg and is best described, as shown here, by a parallel second and third order kinetic scheme. Apparent rate coefficients for this kinetic scheme were determined using cyclic chronopotentiometric data and fitting by digital simulation. A linearization test of computed kinetic rate coefficients versus the number of transitions permits quantitative tests of validity of assumptions made. 相似文献
65.
For some thirty hydrocarbons the s character of hybrids obtained by the application of the maximum overlap method have been correlated with C-H and C-C spin-spin coupling constants. The following relationships were obtained: $$J_{{\text{C}}^{{\text{13}}} - {\text{H}}} = 1079a_{{\text{CH}}}^{\text{2}} /(1 + S_{{\text{CH}}}^{\text{2}} ) - 54.9$$ , $$J_{{\text{C}}_{\text{1}}^{{\text{13}}} - {\text{C}}_{\text{2}}^{{\text{13}}} } = 1020.5a_{{\text{C}}_{\text{1}} }^2 a_{{\text{C}}_{\text{2}} }^{\text{2}} /(1 + S_{{\text{CC}}}^{\text{2}} ) - 8.2$$ . Here the coupling constants are expressed in cps units. In the calculation of the maximum overlap hybrids either the experimental bond lengths or a standard bond lengths were used. For the \(J_{{\text{C}}^{{\text{13}}} - {\text{H}}}\) and \(J_{{\text{C}}^{{\text{13}}} - {\text{H}}} \) coupling constants the standard deviations are 0.9 cps and 1.9 cps respectively. It has been suggested that the large additive constant in the \(J_{{\text{C}}^{{\text{13}}} - {\text{H}}}\) correlation may be attributed to the ionic character of C-H bonds. A good agreement with the experimental data strongly supports the idea that the Fermi contact term and the hybridization are dominant factors in determining carbon-hydrogen and carbon-carbon spin-spin coupling constants across one bond, at least in hydrocarbons. 相似文献
66.
Thermal decomposition of natural siderite and goethite has been studied using Mössbauer spectroscopy and X-ray diffraction. Hematite and magnetite were the principal compounds formed during high temperature treatment of siderite. Natural goethite transformed to hematite at high temperatures. The crystal structures, stoichiometry and the nuclear magnetic properties of Fe-oxides formed are discussed. 相似文献
67.
Novel representatives of the important group of biologically active dibenzosuberone derivatives were prepared: 3,7-dibromo-5-(dimethylaminoethyl- oxyimino)-10,11-dihydro-5H-dibenzo[a,d]cyclohepta-1,4-diene (1), 3,7-dibromo-5-(3- dimethylaminopropylidene)-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (2) and 1,7- dibromo-5-(3-dimethylaminopropylidene)-10,11-dihydro-5H-dibenzo-[a,d]-cycloheptene (3). These compounds are potential tricyclic antidepressants (TCAs), which are still the most frequently prescribed antidepressants in many countries. 相似文献
68.
On the Harary index for the characterization of chemical graphs 总被引:1,自引:0,他引:1
69.
This paper presents qualitative and quantitative comparative results on the simultaneous TG-DTG DTA of five commercial and low-grade bauxites. The methodology of qualitative determination of the basic mineral forms contained in bauxites is currently being established. The weight losses relating to the steps in the TG curve allow determination of the contents of the basic minerals in bauxite. These are recalculated as percentages of Al2O3, SiO2, CaO moisture and total volatiles. The final results are in accordance with the results of classical chemical analyses, and this jusitifies the use of this technique as a quick method for qualitative and quantitative determinations of both commercial and low-grade bauxites.
Zusammenfassung Qualitative und quantitative Ergebnisse vergleichender simultaner TG-DTG-DTA-Untersuchungen an 5 kommerziellen und geringwertigen Bauxiten werden vorgestellt. Die Methodologie der qualitativen Bestimmung der wichtigsten im Bauxit enthaltenen Minerale wird ausgearbeitet. Die Gewichtsverluste bei den entsprechenden TG-Stufen erlauben die Berechnung der Gehalte an den wichtigsten Mineralen. Diese werden umgerechnet in die Anteile an Al2O3, SiO02, CaO, Feuchtigkeit und Glühverlust. Letztere Resultate stimmen mit denen klassisch-chemischer Analyse überein. Das erlaubt die Anwendung thermoanalytischer Methoden als Schnellverfahren für qualitative und quantitative Bestimmungen in kommerziellen und geringwertigen Bauxiten.
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70.
Uniform, well-dispersed silver particles of various morphologies have been prepared by reducing highly acidic silver nitrate solutions with ascorbic acid in the presence of a sodium naphthalene sulfonate-formaldehyde copolymer as dispersing agent. By varying the temperature of the reaction, the free acid content, the addition rate of the reductant, and the aging time, both isometric and anisotropic silver particles could be obtained. It was found that the latter were formed by aggregation of nanosize subunits, which were identified by electron microscopy and X-ray diffractometry. 相似文献