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51.
Grigorii G. Sivets Elena N. Kalinichenko Igor A. Mikhailopulo 《Helvetica chimica acta》2007,90(9):1818-1836
Convergent syntheses of the 9‐(3‐X‐2,3‐dideoxy‐2‐fluoro‐β‐D ‐ribofuranosyl)adenines 5 (X=N3) and 7 (X=NH2), as well as of their respective α‐anomers 6 and 8 , are described, using methyl 2‐azido‐5‐O‐benzoyl‐2,3‐dideoxy‐2‐fluoro‐β‐D ‐ribofuranoside ( 4 ) as glycosylating agent. Methyl 5‐O‐benzoyl‐2,3‐dideoxy‐2,3‐difluoro‐β‐D ‐ribofuranoside ( 12 ) was prepared starting from two precursors, and coupled with silylated N6‐benzoyladenine to afford, after deprotection, 2′,3′‐dideoxy‐2′,3′‐difluoroadenosine ( 13 ). Condensation of 1‐O‐acetyl‐3,5‐di‐O‐benzoyl‐2‐deoxy‐2‐fluoro‐β‐D ‐ribofuranose ( 14 ) with silylated N2‐palmitoylguanine gave, after chromatographic separation and deacylation, the N7‐β‐anomer 17 as the main product, along with 2′‐deoxy‐2′‐fluoroguanosine ( 15 ) and its N9‐α‐anomer 16 in a ratio of ca. 42 : 24 : 10. An in‐depth conformational analysis of a number of 2,3‐dideoxy‐2‐fluoro‐3‐X‐D ‐ribofuranosides (X=F, N3, NH2, H) as well as of purine and pyrimidine 2‐deoxy‐2‐fluoro‐D ‐ribofuranosyl nucleosides was performed using the PSEUROT (version 6.3) software in combination with NMR studies. 相似文献
52.
Analysis of selected ionic liquid cations by ion exchange chromatography and reversed-phase high performance liquid chromatography 总被引:1,自引:0,他引:1
The chromatographic behavior of 8 ionic liquids - 7 homologues of 1-alkyl-3-methylimidazolium and 4-methyl-N-butylpyridinium - has been investigated with a strong cation exchange adsorbent. In particular, the dependence of the retention properties of these solutes on mobile phase composition, pH, and buffer concentration was evaluated with the aim of optimizing and improving the selectivity and retention of solute separation. While using the SCX stationary phase, several interactions occurred with varying strengths, depending on the mobile phase composition. Cation exchange, nonspecific hydrophobic interactions, and adsorption chromatography behavior were observed. Reversed phase chromatography occurred at low concentrations of acetonitrile, electrostatic and adsorption interactions at higher organic modifier concentrations. Elevated buffer concentrations lowered the retention factors without affecting the selectivity of ionic liquids. Obtained results were further compared to the chromatographic behaviour of ionic liquids in the reversed phase system. All analyzed ionic liquids follow reversed-phase behavior while being separated. Much lower selectivity in the range of highly hydrophilic compounds is obtained. This suggests preferred use of ion chromatography for separation and analysis of compounds below 4 carbon atoms in the alkyl side chain. 相似文献
53.
Hong Zheng Wei Yu Hon-bin Zhang Chi-xing Zhou 《高分子科学》2006,(1):1-11
Finite element method is used to simulate the high-speed melt spinning process,based on the equation system proposed by Doufas et al.Calculation predicts a neck-like deformation,as well as the related profiles of velocity,diameter, temperature,chain orientation,and crystallinity in the fiber spinning process.Considering combined effects on the process such as flow-induced crystallization,viscoelasticity,filament cooling,air drag,inertia,surface tension and gravity,the simulated material flow behaviors are consistent with those observed for semi-crystalline polymers under various spinning conditions.The structure change of polymer coils in the necking region described by the evolution of conformation tensor is also investigated.Based on the relaxation mechanism of macromolecules in flow field different types of morphology change of polymer chains before and in the neck are proposed,giving a complete prospect of structure evolution and crystallization of semi-crystalline polymer in the high speed fiber spinning process. 相似文献
54.
Fourier-transform infrared (FTIR) spectroscopy has been a major point of development in many wine laboratories in recent years. It enables almost instant analysis of several properties of wine, usually with very good precision and accurate results. Nevertheless, validation procedures should not be forgotten and should be fully performed. Recovery experiments were performed by spiking wine samples with different amounts of organic acids (tartaric, malic, lactic, acetic and citric—the most prominent in wines). After FTIR analysis of the total acidity and of each organic acid concentration, recoveries were calculated. For total acidity recovery results were, in general, good and very close to 100% (64–111%). On the other hand, for individual organic acid concentrations, the recovery results were lower than 100% (11–73%) for all spiking additions. These results could be explained by spectroscopic interferences between the organic acids. Because they have similar infrared spectra, it is not easy to distinguish between them and, therefore, to achieve accurate calibration. When total acidity, with a different infrared spectrum from the other abundant compounds in the wine, was taken as a single property the recovery results were acceptable. 相似文献
55.
56.
Simutaneous analysis of seven commonly used herbicides, 2,4-D methyl ester, 2,4-D methyl ester, 2,4,5-T methyl ester, silvex methyl ester, ramrod, CIPC and DEF, by gas-liquid chromatography with an electron capture detector was attempted. Two packed columns (which are generally used for the analysis of chlorinated pesticides) and two chemically bonded fused silica capillary columns were used for the analysis. When the packed columns were used, ramrod always interfered with the analysis of 2,4-D methyl ester and/or silvex methyl ester. Complete separation with reasonable analysis time can be achieved using one of the chemically bonded fused silica capillary columns. 相似文献
57.
58.
Summary A preliminary study has been carried out to evaluate a new adsorbent, Thermosorb, for trace level organic contaminants. For this purpose, a comparison was made with a well-characterized adsorbent, Tenax GC, using a prepared aqueous solution of trace organic components. In addition, a comparison was made of chromatograms of air contaminants obtained using both of these adsorbents, under equivalent conditions. The results clearly indicated the potential of this thermally stable, inorganic adsorbent for many trace organic substances of environmental interest. 相似文献
59.
Hydrogen cyanide can be produced by the pyrolysis of man-made polymers. Cyanide has been measured in the blood of healthy adults as well as the blood of fire survivors and fatalities. In healthy subjects the blood cyanide concentration of smokers is higher than that of non-smokers. Fire survivors and fatalities have been found to have higher cyanide levels than of control groups and the levels from fire fatalities are often higher than survivors. Blood concentrations quoted as normal, toxic or fatal are highly variable in the literature. Many studies have been performed to measure the blood cyanide levels in control subjects as well as those who have been exposed to fire but the values found differ. The values for control subjects can vary from none detected to 19 μmol dm−3 while those for fire survivors range from not detected to 150 μmol dm−3 and fatalities range from not detected to 284 μmol dm−3. Analytical techniques and published data are critically reviewed.Many of the existing antidotes for cyanide poisoning are highly toxic themselves and should ideally be administered at doses proportional to the amount of cyanide a patient has received to avoid compounding damage done by cyanide intoxication. For this reason, a rapid, accurate bedside assay of blood cyanide concentration that differentiates between bound and free cyanide would represent a leap forward in the clinical management of cyanide poisoning. 相似文献
60.