排序方式: 共有57条查询结果,搜索用时 15 毫秒
1.
2.
From methyl-5-acetylamino-7,8-anhydro-4,9-O-bis-(t-butyldimethylsilyl)-3,5-dideoxy--D-glycero-D-galacto-2-nonulopyranosidonic acid methylester (1) the derivatives1 a and1 b were obtained by removing the 9-O-(t-butyldimethylsilyl)group withBu
4NF, followed by acetylation. Treatment of1 b with 80% acetic acid and acetanhydride/pyridine yields the 8-epi-N-acetylneuraminic acid derivative2 a and the 7-epi-N-acetylneuraminic acid derivative3 a in a ratio of 3:1 (Scheme 1). The structure elucidation of2 b was achieved by converting2 b via the 4,9-bis-O-(tBDMSi)-8-O-tosyl-derivative2 d into the epoxide1 (Scheme 2). Using the same sequence the epoxides4 and5 were transformed into theN-acetylneuraminic acid derivative6 a and the 7,8-bis-epi-N-acetylneuraminic acid derivative7 a (Scheme 3). After treatment with sodium hydroxide and 0.025m HCl and Dowex 50 H+ the 8-epi-, 7-epi- and 7,8-bis-epi-N-acetylneuraminic acids2,3, and7 were obtained. These three compounds were tested withCMP-N-acetylneuraminic acid synthetase.
Herrn KollegenK. Schlögl mit den besten Wünschen zum 60. Geburtstag. 相似文献
3.
A systematic quantum mechanical study of the possible conformations, their relative stabilities, vibrational and electronic
spectra and thermodynamic parameters of methyl-3-methoxy-2-propenoate has been reported for the electronic ground (S0) and first excited (S1) states using time-dependent and time-independent Density Functional Theory (DFT) and RHF methods in extended basis sets.
Detailed studies have been restricted to the E-isomer, which is found to be substantially more stable than the Z-isomer. Four
possible conformers c′Cc, c′Tc, t′Cc, t′Tc, of which the first two are most stable, have been identified in the S0 and S1 states. Electronic excitation to S1 state is accompanied with a reversal in the relative stability of the c′Cc and c′Tc conformers and a substantial reduction
in the rotational barrier between them, as compared with the S0 state. Optimized geometries of these conformers in the S0 and S1 states are being reported. Based on suitably scaled RHF/6-31G** and DFT/6-311G** calculations, assignments have been provided to the fundamental vibrational bands of both these conformers in terms of frequency,
form and intensity of vibrations and potential energy distribution across the symmetry coordinates in the S0 state. A complete interpretation of the electronic spectra of the conformers has been provided. 相似文献
4.
Paola Mura Gian Piero Bettinetti Maria Teresa Faucci Milena Sorrenti Alessandra Negri 《Supramolecular chemistry》2013,25(4):379-389
Abstract Interactions of naproxen (NAP) with amorphous, randomly methylated β-cyclodextrin at a degree of substitution per anhydroglucose unit of 1.8 (RAMEB) and with crystalline heptakis-(2,6-di-O-methyl)-β-cyclodextrin (DIMEB) were studied in aqueous solution and in the solid state using, respectively, phase-solubility analysis (at 25 °C, 37 °C and 47 °C) and differential scanning calorimetry (DSC) supported by X-ray powder diffractometry. RAMEB and DIMEB displayed similar solubilizing and complexing abilities towards NAP, suggesting analogous inclusion modes of the drug in the host cavity in aqueous solution. Differences were instead observed in interactions in the solid state, where the amorphizing capacity of RAMEB toward NAP (evaluated by DSC) was about twice that of DIMEB at each drug-to-carrier ratio. Assuming that inclusion complexation is also involved in solid-state interactions, molecular modelling accounted for the experimental results in terms of structural features of DIMEB, i.e. the particular inwards orientation of O-6-C-8 groups of three alternate glucoses on the primary hydroxyl side which hampers a deep penetration of NAP in the DIMEB cavity in the solid state. On the contrary, no obstruction of the cavity apparently occurs with RAMEB due its noncrystalline state. The aqueous dissolution rate of NAP from NAP-RAMEB and NAP-DIMEB blends containing 0.59, 0.73, 0.85, and 0.92 mass fraction of carrier linearly increased at decreasing drug-to-carrier ratios. The improvement was 5 to 20 times (from powders) and 50 to 200 times (from discs) the dissolution rate of NAP alone for both carrier. Therefore the choice of the amorphous RAMEB in pharmaceutical formulations can be recommended mainly for economic reasons, though the anhydrous and non-hygroscopic nature of crystalline DIMEB might be of particular advantage in case of moisture sensitive formulations. 相似文献
5.
6.
Synthesis and Characterization of Bis(methyl-2-pyridylmethylidenedrazinecarbodithioate)manganese(II)
Mao-Sheng Liu Qiong-Yan Yu Zheng-Yuan Zhou Qing-Guang Zhan He-Ping Zeng Yue-Peng Cai 《Journal of chemical crystallography》2008,38(11):845-849
Abstract Brown crystals of title compound, bis(methyl-2-pyridylmethylidene-drazinecarbodithioate)manganese(II), was formed by reaction
of methyl-2-pyridylmethylidenehydrazinecarbodithioate(HNNS) with manganese perchlorate at 323 K temperature and recrystallized
from ethanol at room temperature, crystallizing in the monoclinic system, space group P2(1)/n, with a = 11.631(2), b = 14.010(3), c = 13.128(3) ?, β = 105.791(11)°; V = 2058.6(7) ?3, D
c
= 1.533 g/cm3, Z = 4, C16H16N6MnS4, M
r
= 475.53, μ(M0 K
α
) = 1.060 mm−1, F (000) = 972. The structure was refined to R = 0.0441, wR = 0.1196 for 3,682 (I > 2σ(I)) reflections and S = 1.110. In title complex the coordination geometry about manganese is distorted octahedral and the two
ligands in the mer configuration (S and tertiary N atom cis to each other and the iminic N atoms trans). Furthermore, the neutral molecule units MnII(NNS)2 are connected by hydrogen bonds C–H···N and C–H···S and form a three dimensional ordered network structure.
Graphical Abstract The title compound, Mn(NNS)2, exists as discrete molecules in which the central MnII
atom is coordinated by two S atoms and four N atoms from two ligands NNS- molecules
in a mer-octahedral configuration.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
7.
以2-氨基-5-取代苯氧甲基-1,3,4-噻二唑(1)为起始原料, 合成了中间体2-氯乙酰氨基-5-取代苯氧甲基-1,3,4-噻二唑)-2-乙酰亚胺(2)和2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-4-噻唑啉酮(3), 化合物3进一步与取代苯甲醛发生类Knoevenagle缩合反应, 得到了一系列2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-5-(取代苯基亚甲基)-4-噻唑啉酮类化合物4a~4p. 目标化合物4a~4p的结构经IR, 1H NMR和元素分析确证. 相似文献
8.
Roth M 《Journal of chromatography. A》2009,1216(10):1861-1880
Applications and prospects of two-phase, tuneable solvent systems composed of ionic liquids (ILs) and supercritical fluids with an emphasis on supercritical carbon dioxide (scCO(2)) are reviewed. The IL-scCO(2) biphasic systems have increasingly been used in diverse fields of chemistry and technology, and some examples of these applications are mentioned here. Rational design of such applications can obviously benefit from pertinent data on phase equilibria including the partition coefficients of the prospective products and reactants between the two phases. Therefore, a reliable technique to measure the limiting partition coefficients would be of value. Here, the pros and cons of supercritical fluid chromatography in this respect are discussed. An overview of methods for predictive thermodynamic modelling of binary (IL-scCO(2)) and ternary (solute-IL-scCO(2)) systems is also included. 相似文献
9.
利用红外光谱、核磁共振氢谱、紫外光谱以及质谱等表征手段对一种新型蛋白同化激素(AAS)口服药物的主成分进行了研究和鉴定,推定主成分为甲基-1-睾酮(methyl-1-testosterone, M1T, 17β-hydroxy-17α-methyl-5α-androst-1-en-3-one)。在此基础上,建立了M1T的气相色谱-质谱联用检测方法。方法的检出限(信噪比(S/N)为3)为2 ng/mL,定量限(S/N=10)为10 ng/mL;7次平行测定前处理后的加内标尿样的相对标准偏差为9.8%。用该方法测定了该药物在尿样中的排泄曲线。该方法的建立为AAS新药的发现、检测和监控做了很有意义的基础研究工作。 相似文献
10.
K. Ravikumar B. Sridhar M. Mahesh V. V. Narayana Reddy 《Journal of chemical crystallography》2006,36(6):381-387
The crystal structures of isoxazole, 3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]methyl-5-phenyl-,N-oxide] (C13H13N5O3) (I), isoxazole,3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]-methyl-5-(4-methylphenyl)-,N-oxide] (C14H15N5O3) (II) and isoxazole, 3-[[dihydro-2-[(Z)-2-oxohyrazono]-1H-imidazol-1-(3H)-yl]-methyl-5-(2-methoxyphenyl)-,N-oxide] (C14H15N5O4) (III) have been determined by X-ray diffraction studies. The compound I, crystallized in triclinic space group with unit cell dimensions a = 7.2405(7) ?, b = 7.9936(8) ?, c = 11.6573(11) ?, α = 97.801(2)°, β = 90.884(2)°, γ = 96.250(2)° and Z = 2. Compound II crystallized in orthorhombic space group Pna21 with unit cell dimensions a = 10.1778(10) ?, b = 28.228(3) ?, c = 5.1206(5) ?, and Z = 4. Compound III crystallized in monoclinic space group P21/n with unit cell dimensions a = 7.8439(9) ?, b = 7.8544(9) ?, c = 23.534(3) ?, β = 99.464(2)° and Z = 4. For all three compounds, the five-membered imidazolidine ring adopts an envelope conformation. The crystal structures are stabilized by both the intramolecular N–H···O and intermolecular N–H···N hydrogen bonding. 相似文献