共查询到20条相似文献,搜索用时 140 毫秒
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以离子液体为催化剂,由维生素E经两步酯化反应合成了聚乙二醇1000(PEG1000)维生素E琥珀酸酯。以离子液体1-(N',N'-二甲胺乙基)-3-甲基咪唑四氟硼酸盐为催化剂、1,2-二氯乙烷为助溶剂、维生素E与琥珀酸酐摩尔比为1:1.2,在80 ℃条件下反应4 h,维生素E琥珀酸酯(TAS)的产率为90%。以1-丙磺酸基-3-甲基咪唑硫酸氢盐/甲苯为反应体系,TAS与PEG1000摩尔比为1:2,在100 ℃下反应5 h,PEG1000维生素E琥珀酸酯(TPGS)收率为91%。 相似文献
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以D-葡萄糖为原料,经碳苷化反应,酰化反应和脯氨酸-DIPEA催化的aldol反应制得2个碳苷糖[1-(4'-羟基苯基)-4-C-β-四乙酰基葡萄糖基-3-烯-2-酮(5a)和1-(3-羟基苯基)-4-C-β-四乙酰基葡萄糖基-3-烯-2-酮(5b)];5与琥珀酸维生素D2经Steglich酯化反应合成了2个新型碳苷糖类维生素D2衍生物,其结构经1H NMR,13C NMR和HR-ESI-MS表征。 相似文献
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2-氧代-6-甲基庚酰基三尖杉碱(3)与0-(1-甲氧基异丙基)羟基乙酸甲酯(4)在强碱性试剂二异丙胺锂(LDA)存在下,起亲核加成反应,反应中间体5在室温用酸性丙酮水解,得到一种新的三尖杉酯类生物碱一一高异三尖杉酯碱(6c)及其立体异构体(6a、6b、6d)的混合物,产率56%、通过制备薄层层析分得这四个立体异构体,它们的1H NMR和异三尖杉酯碱及其立体异构体的1H NMR类似,推定了它们的绝对构型。初步药理试验表明,高异三尖杉酯碱及其立体异构体的混合物对白血病L7712的DNA合成有明显的抑制作用。 相似文献
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以廉价的异香草醛和2,4,6-三羟基苯乙酮为起始原料,经过C-异戊烯基化、选择性甲基化、甲氧甲基化、羟醛缩合、去保护基、催化环化以及脱除甲基等步骤,分别以13.3%和23%的总收率首次完成了天然异戊烯基黄烷酮Glovanon(1)和5-O-methylglovanon(2)的全合成.合成的关键步骤是2,4,6-三羟基苯乙酮的单C-异戊烯基化.所有新化合物的结构都经过1H NMR,IR,MS确认.抑菌活性研究表明,两种新合成的化合物对藤黄微球菌(M.luteus)和大肠杆菌(E.coli)均有良好的抑制作用. 相似文献
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Lorenzo Tattini Pierandrea Lo Nostro Luca Scalise Barry W. Ninham Piero Baglioni 《Journal of colloid and interface science》2009,339(1):259-265
Diblock semifluorinated n-alkanes can form aggregates and gels in fluorinated solvents. We have investigated the thermal behavior of binary mixtures comprising F(CF2)8(CH2)16H and fluorinated solvents. The solvents were perfluorohexane, perfluoroheptane, perfluorooctane, perfluorooctyl bromide, perfluorodecalin, and perfluorotributylamine. The phase diagrams were used to calculate the activity coefficients of the two components and the main excess thermodynamic functions. The solubility and self-assembly behavior of F8H16 in the fluorinated solvents are related to the different solute–solvent dispersion interactions that depend on the polarizabilities and ionization potentials of the interacting species, and on the structural properties of the solvent. 相似文献
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Martyna Rzelewska-Piekut Zuzanna Wiecka Magdalena Regel-Rosocka 《Molecules (Basel, Switzerland)》2022,27(2)
The paper presents basic studies on the precipitation of platinum, palladium, rhodium, and ruthenium nanoparticles from model acidic solutions using sodium borohydride, ascorbic acid, and sodium formate as reducing agents and polyvinylpyrrolidone as a stabilizing agent. The size of the obtained PGM particles after precipitation with NaBH4 solution does not exceed 55 nm. NaBH4 is an efficient reducer; the precipitation yields for Pt, Pd, Ru, Rh are 75, 90, 65 and 85%, respectively. By precipitation with ascorbic acid, it is possible to efficiently separate Pt, Rh, and Ru from Pd from the two-component mixtures. The obtained Pt, Pd, and Rh precipitates have the catalytic ability of the catalytic reaction of p-nitrophenol to p-aminophenol. The morphological characteristic of the PGM precipitates was analyzed by AFM, SEM-EDS, and TEM. 相似文献
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采用密度泛函理论(DFT)以及广义梯度近似方法(GGA)计算了甲酸根(HCOO)在Cu(110)、Ag(110)和Au(110)表面的吸附. 计算结果表明, 短桥位是最稳定的吸附位置, 计算的几何参数与以前的实验和计算结果吻合. 吸附热顺序为Cu(110)(-116 kJ·mol-1)>Ag(110)(-57 kJ·mol-1)>Au(110)(-27 kJ·mol-1), 与实验上甲酸根的分解温度相一致. 电子态密度分析表明, 吸附热顺序可以用吸附分子与金属d-带之间的Pauli 排斥来关联, 即排斥作用越大, 吸附越弱. 另外还从计算的吸附热数据以及实验上HCOO的分解温度估算了反应CO2+1/2H2→HCOO的活化能, 其大小顺序为Au(110)>Ag(110)>Cu(110). 相似文献
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The tripodal ligand 4-(2′-pyridylmthyl)-4-azaheptane-1,7-diamine has been prepared by reaction of 2-aminemethyl pyridine with acrylonitrile, followed by the reduction of the nitrile groups. Copper(II), nickel(II), zinc(II), cobalt(III) and chromium(III) complexes of the ligand have been prepared and characterized and the crystal structures of the complexes [CuLCl]ClO4 and [NiL(MeCN)2](ClO4)2 determined. The copper complex is five coordinate with approximate square pyramidal stereochemistry with the apical position occupied by a primary amine donor. The nickel complex is octahedral with the pyridine nitrogen donor lying trans to an acetonitrile ligand. 相似文献
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《Journal of Coordination Chemistry》2012,65(1-2):173-182
Abstract The reaction, in water, of Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) ions with sodium ampicillinate at room temperature has allowed isolation of dimers with the following general formula [M(amp)Cl]2 × nH2O (n = 1.5?3.2). The complexes were characterized by elemental analyses, conductivity measurements, magnetic susceptibilities and spectroscopic methods (IR, Raman, EPR and UV-Visible). A dinuclear structure based on octahedrally coordinated metal ions is proposed. 相似文献
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Coordination compounds based on imidazole and benzimidazole substituted nitronyl nitroxide radicals with transition metal ions and trivalent lanthanide ions are described from the perspective of their magnetic properties.For the transition metal compounds the crystal structures show various metal-nitroxide dimensionalities including mononuclear (0D), one-dimensional (1D) and two-dimensional (2D) complexes. The mononuclear complexes were isolated with most metal ions of the first transition series. One copper(II) complex shows a copper(II)-radical ferromagnetic coupling (J = +75 cm−1) while for the other mononuclear compounds, mainly with manganese(II), the metal-radical interactions are antiferromagnetic. The one-dimensional and two-dimensional complexes are manganese(II) compounds which show canting effects leading to weak ferromagnetism.For the trivalent lanthanide ions [La(III), Gd(III) and Eu(III)], three series of mononuclear complexes were obtained in which the metal center is bound to four, two or one nitroxide radicals depending on the counter ions and ancillary ligands. Unexpectedly, in most gadolinium(III) complexes, the Gd(III)-radical interactions were found to be antiferromagnetic in contradiction with other foundings and previous theoretical models. In support to the magnetic studies, the optical properties of the lantanide complexes have also been investigated and are briefly described. 相似文献
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A selective and sensitive reagent of 2-pyridine carboxaldehyde isonicotinyl hydrazone(2-PYAINH) was synthesized and studied for the spectrophotometric determination of nickel, copper, cobalt, and iron in detail. At a pH value of 7.0, 9,0, 9.0, and 8.0, respectively, which greatly increased the selectivity; nickel, copper, cobalt, and iron reacted with 2-PYAINH to form a 1:2 yellow-orange, 1:2 yellow-green, 1:2 yellow and 1:1 yellow complexes, with absorption peaks at 363, 352, 346, and 359 nm, respectively. Under the optimal conditions, Beer's law was obeyed over the ranges of 0.01-1.4, 0.01-1.5, 0.01-2.7, and 0.01-5.4 mg/L respectively. The apparent molar absorptivity and Sandell's sensitivities were 8.4×10^4, 5.2×10^4, 7.1×10^4, and 3.9×10^4 L·mol^-l·cm^-1, respectively, and 0.00069, 0.0012, 0.00078, and 0.0014 μg·cm2, respectively. The detection limits were found to be 0.001, 0.002, 0.003, and 0.01 mg/L, respectively. The detailed study of various interfering ions to make the method more sensitive was carried out and selective and several real samples were analyzed with satisfactory results. 相似文献
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Alberto Cassol Plinio Di Bernardo Pier Luigi Zanonato Sergio Tamburini Patrizia Tomasin Pietro Alessandro Vigato 《Supramolecular chemistry》2013,25(3):469-488
Abstract The asymmetric compartmental macrocycles containing one N2O2 or N3O2 Schiff base and one O2O3 or O2O4 crown-ether like chamber, have been obtained by condensation reaction of the formyl precursors 3,3′-(3-oxapentane-1, 5-diyldioxy) bis (2-hydroxybenzaldehyde) or 3,3′-(3,6-dioxaoctane-1,8-diyldioxy)-bis(2-hydroxybenzaldehyde) with ethyl ethylenediamine (H2LA, H2LC), 1,5-diamino-3-azamethylpentane(H2LB, H2LD), also in the presence of metal ions as templating agents. These ditopic ligands, with dissimilar coordination sites, have been designed and used for the selective complexation of “d” and/or “s” metal ions, respectively into the Schiff base and the crown ether chamber. The selectivity of these processes strongly depends on the size and on the donor atom sets of the sites. The possibility to obtain mononuclear M(L)·nH2O (M = Ni2+, Cu2+, Co2+), Mn(L)(CH3COO)·nH2O or Na(L) and hetero-dinuclear MNa(L)(CH3COO) (M = Ni2+, Cu2+, Co2+) and MnNa(L)(CH3COO)2·nH2O complexes has been successfully tested. The ligands and complexes have been characterized by ir, nmr, mass spectrometry and magnetic susceptibility measurements. Two of the ligands used for the preparation of the solid samples, i.e., to H2LA and H2LB, have been employed to study complexation reactions of Co(II) and Na(I) in solution. In order to obtain information on the ligand preorganization effect toward the complex stabilities, a simpler open chain parent compound of H2LB (H2LE) has been also prepared and studied. FT-IR spectra show that H2LA is unable to complex Na+ in DMSO while the complexation reactions of Na+ by H2LB and of Co2+ by H2LA take place with slow kinetics. Therefore, thermodynamic data have been obtained only for the systems Co2+/H2LB and Co2+/H2LE. The thermodynamic parameters obtained for the complexation reactions show that the pre-organization of the donor atoms in H2LB does not add a significant contribution to the stabilities of the complexes. Both H2LB and H2LE form in DMSO 1:1, 1:2 and 1:3 = M:L complexes with very similar stabilities and almost equal enthalpies of formation. Physico-chemical studies suggest besides that the slow reaction of Na+ with H2LB is probably due to the formation of a 1:1 complex where the metal cation, initially occupying the O3 cage of the ligand, slowly binds also the oxygens of the phenolic moieties. Spectral and calorimetric data on solutions containing H2LB and different Co2+: Na+ ratios evidence that in DMSO no stable heterodinuclear complexes form when the neutral ligand is considered. 相似文献