N—BOC—8—氨甲基—2—萘甲酸的改进合成法

以２－萘甲酸为原料，经硝化，酯化，重氮化，选择性催化氢化，ＢＯＣ酸酐保护等六步反应，完成了Ｎ－ＢＯＣ－８氨甲基－２－萘甲酸（１ａ）的合成，为化合物１的合成提供了新的合成途径。     

A Two-dimensional Lanthanide Coordination Framework with a New Amide-type Tripodal Ligand, 2,2′,2＂-Nitrilotris{[（2′- benzylaminoformyl）phenoxy]ethyl}amine

The La(III) complex with a new amide‐type tripodal ligand,2,2′.2″‐nitrilotris{[(2′‐benzylaminofomyl)‐phenoxylethyl)amine (L), was synthesized and characterized by X‐ray crystallographic analysis. Crystal data: C₄₈H_55.50LaN₇O_18.75, M_r=1169.40, monoclinic. space group, P2₁/n, a= 1.0644(3) nm. b=2.3889(5) nm, c= 2.1917(5) nm, β=90.65°, V=5.573(2) nm³, Z=1, D_c=1.394 g°cm^?3, R₁=0.0487, wR [1>2s?(I)]=0.1266. The results reveal that each La(III) ion binds to 9 oxygen atoms, three of which belong to carbonyl groups from three tripodal ligands and six to three bidentate nitrate groups and a two‐dimensional sheet of 4.8² networks is assembled by metal‐ligand coordination interaction. L, a heptadentate compound, merely acts as a tridentate bridging spacer due to its steric hindrance and links the La(III) ions as three‐connected nodes.     

反相液体色谱中饱和醇保留行为的研究 Ⅰ.低碳醇保留行为与溶质分子结构的关系

本文从吸附-疏溶剂理论出发,根据热力学平衡观点,导出了一定固定相和流动相时,描述溶质保留行为与其分子结构关系的理论模型,并用之预测了饱和醇的保留值,获满意结果。从而表明本模型不但能用于同系物,而且亦可用于同分异构体及立体异构体保留行为的预测。     

Spectroscopic characterization of effective components anthraquinones in Chinese medicinal herbs binding with serum albumins

The interactions of serum albumins such as human serum albumin (HSA) and bovine serum albumin (BSA) with emodin, rhein, aloe-emodin and aloin were assessed employing fluorescence quenching and absorption spectroscopic techniques. The results obtained revealed that there are relatively strong binding affinity for the four anthraquinones with HSA and BSA and the binding constants for the interactions of anthraquinones with HSA or BSA at 20 degrees C were obtained. Anthraquinone-albumin interactions were studied at different temperatures and in the presence of some metal ions. And the competition binding of anthraquinones with serum albumins was also discussed. The Stern-Volmer curves suggested that the quenching occurring in the reactions was the static quenching process. The binding distances and transfer efficiencies for each binding reactions were calculated according to the F?ster theory of non-radiation energy transfer. Using thermodynamic equations, the main action forces of these reactions were also obtained. The reasons of the different binding affinities for different anthraquinone-albumin reactions were probed from the point of view of molecular structures.     

Theoretical study of the reaction of Sc with SCO in gas phase

In order to elucidate the mechanism of reaction M⁺ + SCO, both triplet and singlet potential energy surfaces (PESs) for the reaction of Sc⁺ + SCO have been theoretically investigated using the DFT (B3LYP/6-311+G*) level of theory. The geometries for reactants, intermediates, transition states and products were completely optimized. All the transition states were verified by the vibrational analysis and the intrinsic reaction coordinate calculations. The involving potential energy curve-crossing dramatically affects reaction mechanism, reaction rate has been discussed, and the crossing points (CPs) have been localized by the approach suggested by Yoshizawa et al. The present results show that the reaction mechanism are insertion–elimination mechanism both along the C–S and C–O bond activation branches, but the C–S bond activation is much more favorable in energy than the C–O bond activation. All theoretical results not only support the existing conclusions inferred from early experiment, but also complement the pathway and mechanism for this reaction.     

Fabrication of hexaphenylsilole nanowires and their morphology-tunable photoluminescence.

Immersion of nanoporous alumina membranes into saturated solutions of hexaphenylsilole with subsequent solvent evaporation affords aligned organic nanowires. The luminescent properties of the hexaphenylsilole nanowires can be manipulated by varying their morphologies, which were controlled by changing the channel sizes of the alumina templates.     

细胞色素C的电化学行为研究

本文评述了细胞色素Ｃ电化学研究的发展概况，重点介绍了细胞色素Ｃ在促进剂作用下的电化学行为，促进剂种类，影响促进作用的因素及促进机理。     

甲苯胺蓝指示反应动力学光度法测定痕量钌

在磷酸和热水浴中 ,钌 (Ⅲ )对高碘酸钾氧化甲苯胺蓝的反应具有催化作用 ,据此建立了测定钌的新催化光度法。钌在 0～ 0 .0 5 0 μg/ 2 5ml范围内与催化反应速率有良好的线性关系 ,检出限为 5 .5 3× 10 - 5μg·ml- 1。对 0 .0 30 μg/ 2 5ml钌 (Ⅲ )测定的相对标准偏差为 2 .0 % (n =11)。该催化反应对钌 (Ⅲ )和甲苯胺蓝分别为一级反应 ,其表观活化能为 5 0 .2 6kJ·mol- 1。试验了 4 0多种共存离子的影响 ,大多数的常见离子不干扰。该方法用于岩矿和冶金产品中钌的测定 ,相对标准偏差为 2 .1%～ 2 .4 % ,标准加入回收率为 10 0 .1%～ 10 5 .4 %。     

Strong influences of cocatalyst on ethylene/propylene copolymerization with a MgCl2/SiO2/TiCl4/diester type Ziegler-Natta catalyst

Using triethylaluminum (TEA), triisobutylaluminum (TIBA) or TEA/TIBA mixtures of molar ratio 75/25, 50/50 and 25/75 as the cocatalyst, five different ethylene-propylene copolymer samples were synthesized by a MgCl₂/SiO₂/TiCl₄/diester type Ziegler-Natta catalyst in a slurry polymerization process. The synthesized copolymers are strongly heterogeneous in chain structure and were fractionated into part of nearly random copolymer and part of segmented copolymer. Both polymerization activity and copolymer structure were found to be markedly changed when the cocatalyst was changed from TEA to TEA/TIBA mixtures or pure TIBA. As the content of TEA in cocatalyst increases, yield of the random part of product increases and the yield of the crystalline segmented copolymer part decreases. There is also a decrease in ethylene content of the whole product with increasing TEA amount. Copolymerization behaviors of the TEA/TIBA mixture activated catalysis systems are not simple superposition of those activated by pure TEA and TIBA. When a 50/50 TEA/TIBA mixture was used as cocatalyst, the copolymerization activity became the highest, and yields of both the random copolymer part and the segmented copolymer part are close to the highest level. On the other hand, both parts of the copolymer produced with a 50/50 TEA/TIBA mixture are relatively more blocky than the products of TEA or TIBA systems, and difference in ethylene content between the random part and the segmented part was the smallest. The segmented copolymer part of three typical samples was further fractionated by temperature-gradient extraction fractionation into fractions of different ethylene content and sequence distribution. Changing TEA content in the cocatalyst exerted strong influences also on the fraction distribution of the segmented part of copolymer.     

Synthesis and Characterization of Novel Orange-emitting Iridium（Ⅲ） Complexes with Diphenylquinoline Ligands Containing Fluorinated Substituent

Three new cyclometalated iridium（m） complexes based on ligands of diphenylquinoline with fluorinated subsfituents were prepared, and characterized by elemental analysis （EA）, ^1H NMR, and mass spectroscopy （MS）. The photophysical and electrophosphorescent properties of the complexes were briefly discussed.