用于同步辐射光源的成像板粉末衍射系统

报道了我们研制的一套成像板粉末衍射装置,对其误差来源进行了详细的分析讨论,并与衍射仪进行了比较.该装置的半径为143.3mm,最大测量角度范围不160°，最大角度(2q )偏差小于0.03°,这些性能指标已被实验所证实,完全可应用于粉末衍射全谱的测量.     

糖类研究（XXXI）：带连接臂的乳糖衍生物及二聚体的合成

八乙酰乳糖与一缩二乙二醇或二缩三乙二醉承ＢＦ３．Ｅt２Ｏ催化下反应生成相应的β－ 糖苷,后者在同样的催化剂存在下再与八乙酰乳糖反应生成对称的β－构型二聚体。糖苷与二聚体在甲醇钠／甲醇溶液中脱去乙酰基生成目标化合物用于抗癌转移活性研究。     

低共熔混合锂盐相图的绘制及应用

采用热分析法对不同组成的混合锂盐二元体系进行研究, 绘制了混合锂盐体系的步冷曲线和T-x相图, 结果表明体系均为具有最低共熔点的二元体系. LiOH-LiNO3、LiOH-LiCl、LiOH-Li2CO3及LiNO3-LiCl体系的最低共熔点分别为175.7、294.5、418.2及221.6 ℃. 利用低共熔混合物LiNO3-LiOH为锂盐与不同前驱体反应, 制备出了层状结构良好的锂离子电池正极材料LiNiO2、LiNi0.8Co0.2O2及LiNi1/3Co1/3Mn1/3O2. X射线衍射分析表明, 合成的材料具有规整的层状NaFeO2结构, 且XRD衍射峰强度之比I(003)/I(104)>2.0, 电性能测试表明, 在2.7-4.3 V(vs Li/Li+)的电压范围内进行0.1C倍率充放电, LiNiO2、LiNi0.8Co0.2O2、LiNi1/3Co1/3Mn1/3O2首次充电比容量分别达168.0、225.4、194.0 mAh·g-1, 放电比容量分别为138.4、165.8、157.7 mAh·g-1.     

A new isocoumarin from bark of Pellodendron chinense

A new isocoumarin, 3-acetyl-3,4-dihydro-5,6-dimethoxy-1H-2-benzopyran-1-one, was isolated from the cortex of Phellodendron chinense schneid. The structure was determined on the basis of spectroscopic evidences.     

微波干法催化芳香醛与绕丹宁及N-苯基绕丹宁的缩合反应

利用微波辐射和固体碱性载体试剂催化绕丹宁及N-苯基绕丹宁和芳香醛的缩合反应合成了14个绕丹宁衍生物并研究了影响反应的因素。     

An efficient ionic liquid supported divergent assembly of 3,6-branched glucosamine-containing pentasaccharide

We utilized the glycosyl acceptor tagging method with ionic liquid support for synthesis of the core segment of Clostridium botulinum C2 toxin ligand through a divergent synthetic strategy without chromatographic purification.The total yield was 57.1% and the reaction was completed in 10 h.The efficient ionic liquid supported glycosylation and purification procedure was applied for the synthesis of branched glucosamine-containing oligosaccharides for the first time,which expanded the scope of ionic liquid supported synthesis of biologically important oligosaccharides.     

Synthesis, Spectroscopic Properties and Crystal Structural Characterization of a Triphenyltin(Ⅳ) Complex with 5-Bromonicotinic Acid

A novel organotin complex [Ph3Sn(C2H5OH)(OCOC5H3NBr)SnPh3(OCOC5H3NBr)]has been synthesized by the reaction of 5-bromonicotinic acid with triphenyltin hydroxide in ethanol and characterized by elemental analysis, IR and 1H NMR. The crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 15.564(2), b = 24.975(4), c = 12.2973(19) (A), β = 92.224(2)°, Z = 4, V = 4776.5(13) (A)3, Dc = 1.596g/cm3, μ(MoKα) = 2.765 mm-1, F(000) = 2264, R = 0.0385 and wR = 0.0667. In the molecular structure of the title complex, the tin atoms are five-coordinated in a trigonal bipyramidal geometry.     

Efficient synthesis of a series of novel fructose-based 3-acetyl-5-alkyl-2,3-dihydro-1,3,4-oxadiazole derivatives and studies of the reaction mechanism

A series of novel alkyl substituted fructose-based oxadiazoles were synthesized and their cytotoxic activities toward tumor cells were investigated. We studied the reaction mechanism and the stereochemistry of the reaction. Tautomerization between isomers 2 and 3 was observed in solution. The tautomerization was accelerated by heating or in the presence of acetic acid. An intermediate 6 during the heterocyclization was isolated, and two different pathways for the heterocyclization were suggested. On the basis of these findings, an efficient method, with the assistance of microwave irradiation was developed for the synthesis of 4 and 5. The yields were satisfactory and no by-products were found. We also proposed that the (R/S)-configurations of oxadiazoles were determined by the E/Z configurations of hydrazones.     

GISAXS and SAXS studies on the spatial structures of Co nanowire arrays

The spatial structures of magnetic Co nanowire array embedded in anodic aluminium membranes were investigated by grazing incidence small angle X-ray scattering (GISAXS) and conventional small angle X-ray scattering (SAXS) techniques. Compared with SEM observation, the GISAXS and SAXS measurements can get more overall structural information in a large-area scale. In this study, the two-dimensional GISAXS pattern was well reconstructed by using the IsGISAXS program. The results demonstrate that the hexagonal lattice formed by the Co nanowires is distorted (a ≈ 105 nm, b ≈ 95 nm). These Co nanowires are isolated into many structure domains with different orientations with a size of about 2 μm. The SAXS results have also confirmed that the nanopore structures in the AAM can be retained after depositing Co nanowires although the Co nanowires can not completely but only just fill up the nanopores. These results are helpful for understanding the global structure of the Co nanowire array.