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201.
Dzygiel A Rzeszotarska B Masiukiewicz E Cmoch P Kamieński B 《Chemical & pharmaceutical bulletin》2004,52(2):192-198
Methyl 5-amino-1H-[1,2,4]triazole-3-carboxylate hydrochloride (1). and free ester (2). were obtained and 2 was reacted with Ac(2)O to give the acetylated products 3-6. Compounds 1-6 were studied using HPLC, GC-MS, FTIR and multinuclear NMR spectroscopy, including the cross-polarisation magic angle spinning (CPMAS) technique. The results of the acetylation of 2 were compared to those of the acetylation of 5-amino-1H-[1,2,4]triazole, and for 2 a significant decrease in the susceptibility to acetylation was found. The reaction of 2 with Ac(2)O at 20 degrees C, regardless of the amount and the concentration of the latter, including neat Ac(2)O, proceeds fully regioselectively and leads to one product: methyl 1-acetyl-5-amino-1H-[1,2,4]triazole-3-carboxylate (3). In sharp contrast to 5-amino-1H-[1,2,4]triazole, neither an additional monoacetylated isomer, whether annular or exocyclic, nor any diacetylated derivative could be detected. The diacetylation of 2 requires the process to be carried out in neat boiling Ac(2)O and, as in the case of 5-amino-1H-[1,2,4]triazole, gives two diacetylated isomers. These are methyl 1-acetyl-3-(acetylamino)-1H-[1,2,4]triazole-5-carboxylate (4) and 1-acetyl-5-(acetylamino)-1H-[1,2,4]triazole-3-carboxylate (5). Hypothetical pathways of their formation have been suggested. A mixture of 4 and 5 upon hydrolysis of the ring acetyl group gives the monoacetylated derivative methyl 5-(acetylamino)-1H-[1,2,4]triazole-3-carboxylate (6). The spectroscopic, structural and conformational characteristics of compounds 1-6 have been given and methods for their preparation have been provided. 相似文献
202.
Krystyna Cieśla H. Rahier Grażyna Zakrzewska-Trznadel 《Journal of Thermal Analysis and Calorimetry》2004,77(1):279-293
One to three endothermal peaks atributted to melting of bulk and interfacial water were observed by DSC in the regenerated
cellulose — water system. The profiles of thermal effects depend on water content, time of conditioning, film pretreatment
and the conditions applied during the preceding freezing-thawing cycles. The occurrence might be deduced of melting-crystallisation
processes. A large amount of non-freezable strongly bounded water was also detected.
Although cellulose absorbs water quickly after immersion, the structural changes consisting on ordering of polymer fraction
occur during further conditioning due to increase in strength of water binding. Using the membranes in the separation module
at 90°C causes weakening of these bonds. Differences between interaction of particular cellulose films with water can be detected
during the first, the second and the third heating.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
203.
Anna Kowalska Zygmunt Kowalski Andrzej Kotarba Andrzej Barański 《Mikrochimica acta》1990,100(5-6):349-353
The analytical procedure of determination of Fe(II) in the presence of Fe(III) in milligram samples is proposed. A solid sample is dissolved in hydrochloric acid in argon atmosphere. Subsequently, the pH-value of the solution is fixed and Fe(III) complexed by phosphoric buffer. At the next step Fe(II) is oxidized by -molybdosilicic acid. Finally, the intensity of colouring caused by the reduced form of the acid is measured at the wavelength 770 nm. The proper treatment of the sample during oxidation, and immediately before, is decisive for the accuracy of the analysis. The method was verified by means of the analysis of synthetic magnetite. The theoretical content of Fe(II) was 24.12%, the determined one was 24.02 ± 0.10%. The method was applied to the determination of the homogeneity of an iron catalyst for ammonia synthesis. 相似文献
204.
Summary
This paper is dedicated to the study of Hilbert functions and Betti numbers of the projective varieties in a flat family. We prove that the Hilbert function H(X
y
,n),y Y-a parameter scheme-is lower semicontinuous for any fixed n. In case Y is integral and noetherian we obtain the well-known fact that the set V Y where H(X
y
,n)is maximal for all n's is open and nonempty. We show also that bi(X
y
)-the i- th Betti number of Xy—is upper semicontinuous for y V. The paper contains also a number of results concerning the relations among the various Betti numbers.Member of G.N.S.A.G.A.-C.N.R. Supported in part by M.P.I. (Italian Minstry of Education). 相似文献
205.
M. Ježabek J. Karczmarczuk M. Rożańska 《Zeitschrift fur Physik C Particles and Fields》1985,29(1):55-60
In the framework of the dual parton model we calculate the spectra of secondary antibaryons in \(\bar p\) -nucleus non-annihilation inelastic interactions. We find that the number of antibaryons in the backward hemisphere in the \(\bar p\) -nucleon centre-of-mass frame can grow with the atomic number of the nucleus. 相似文献
206.
The anomalous temperature dependence of the elastic constantsc
11 andc
66 and the elastic instability temperatureT
c are obtained in the two-dimensional microscopic model of the alkali cyanides crystals. It has been found, by means of the Michel and Naudts' theory of the translation rotation coupling, that the orientational disorder in the high-temperature phase leads to the critical softening of the shear elastic constantc
66. 相似文献
207.
An HPLC procedure for determination of phenoxyalkanoic acid herbicides in water samples is proposed. The analytical column Phenomenex C18(2) Luna 5 µm and UV detection at 225 nm were applied. Baseline resolution was achieved in isocratic mode with a mobile phase consisting of acetonitrile/acetic acid (40/60, v/v), adjusted to pH 2.5. SPE sorbents – C18 BondElut, phenyl-silica, LiChrolut SAX and polymeric sorbents – were compared for isolation and preconcentration of 6 phenoxyalkanoic acid herbicides. Higher (above 95%) and more reproducible recoveries were obtained with polymeric and phenyl-silica sorbents using pure methanol for elution. The method was tested for river water samples with the limit of detection in the range of 2–3 µg L−1 (for 50 mL sample) and a reproducibility of 5% RSD. 相似文献
208.
The strategy to identify cadmium deactivation mechanism in Arabidopsis thaliana has been developed using selective and sensitive hyphenated techniques. Cadmium concentrations, in main parts of the plant, were determined by ICP-MS and total amount was found as 0.43-0.44 μg g−1 in leaves and 3.3-3.4 μg g−1 in roots. Speciation of the metal complexes in cells was investigated by SEC-ICP-MS in order to estimate the accumulation process. Phytochelatins, desglycyl-phytochelatins and phytochelatins homologues lacking the N-terminal γ-linked glutamic acid were extracted from plant and were identified by RPLC-ESI-MS. Two-dimensional chromatography allowed to link the metal complexes separated by SEC with isoforms of phytochelatins analyzed by high resolution RPLC and confirm their significant responsibility for metal accumulation. The potential of the cadmium complexes speciation indicates that obtained results could be reliable source of knowledge to confirm the information coming from the well-known genomic sequence of Arabidopsis and to estimate the role of γ-glutamyl transpeptidase in metabolism of glutathione. 相似文献
209.
铱(Ⅲ)与2-(5-溴-2-吡啶偶氮)-5-二甲氨基苯胺的显色反应及其应用 总被引:1,自引:0,他引:1
研究了试剂2_(5_溴_2_吡啶偶氮 )_5_二甲氨基苯胺 (5_Br_PADMA)与铱 (Ⅲ )的显色反应 ;在 pH4.75~6.00的HAc -NaAc缓冲溶液中 ,铱 (Ⅲ )与5_Br_PADMA形成摩尔比为1∶2型稳定的红色络合物 ,在0.6mol/LH2SO4溶液中 ,其最大吸收波长为558nm ,表观摩尔吸光系数为5.1×104L/(mol·cm) ,铱 (Ⅲ )含量在0~0.8mg/L范围内符合比尔定律 ,采用加入适量EDTA的方法消除了Fe3 + 、Co2 + 、Ni2 + 等干扰离子 ,建立了在二元络合物体系中测定微量铱 (Ⅲ )的灵敏度高、选择性好、简便、稳定的分光光度法 相似文献
210.
W. Bocian J. Jaźwiński O. Staszewska J. W. Wiench L. Stefaniak G. A. Webb 《Chemistry of Heterocyclic Compounds》1996,32(11-12):1358-1366
Multinuclear1H,13C,14N,15N, and17O NMR data are presented for some sydnones, isosydnones and isothiosydnones. The type of valence tautomerism shown in (Fig. 1) is not observed for the compounds studied. At high pH compounds2 and12 are found to undergo transformations. The more suitable NMR parameters are reported for establishing the structures of mesoionic compounds containing three heteroatoms in the five-membered conjugated ring. Someab initio GIAO calculations on a model structure of sydnones and related compounds have been performed. 相似文献