Fluorous Synthesis of Biaryl-Substituted Proline Analogs by 1,3-Dipolar Cycloaddition and Suzuki Coupling Reactions

A solution-phase synthesis of bicyclic prolines containing four points of diversity has been developed by a two-step synthesis involving 1,3-dipolar cycloaddition of perfluoroalkylsulfonyl-protected hydroxybenzaldehydes followed by Pd-catalyzed Suzuki coupling reaction of fluorous sulfonates with boronic acids. Both reactions are conducted under microwave irradiation and reaction mixtures are purified by solid-phase extractions without performing chromatography.     

Determination of mercury in human urine by neutron activation analysis,with lead diethyldithiocarbamate as a preconcentration agent

Lead diethyldithiocarbamate is an effective reagent for preconcentration of mercury in urine for neutron activation analysis. Sodium and bromine are removed from the sample by this procedure. As lead diethyldithiocarbamate is insensitive to neutron activation, radiochemical separation is not needed after neutron irradiation. Results from the analysis of urine collected from workers in caustic soda manufacturing plants are discussed.     

TiO_2-CeO_2催化剂湿式氧化苯酚的活性研究

采用共沉淀法制备了湿式氧化降解苯酚的TiO2-CeO2催化剂,测定了反应过程中不同反应时间的COD去除率,结果表明,当Ti、Ce摩尔比为3∶1时,在150℃、总压5MPa(其中氧分压4.5MPa)时,所制备的催化剂活性最高,反应90分钟COD去除率可以达到71%.对催化剂进行了比表面积、XRD和XPS测试,结果表明,高效的催化剂具有较多的活性位、催化剂粉末体系Ce的变价特性以及大量的表面吸附氧.     

催化动力学光度法间接测定水中痕量硫离子

在氨水介质中,硫离子可阻抑Fe(Ⅲ)催化过氧化氢氧化二甲酚橙褪色,并且催化体系和阻抑体系在570 nm处吸光度的差值与硫离子浓度呈线性关系,据此建立了阻抑动力学光度法间接测定痕量硫离子的新方法。方法的线性范围为0.0020~0.044mg/L,检出限为1.6×10-9g/mL,对0.040 mg/L硫离子进行10次平行测定的相对标准偏差为2.1%。方法用于废水中硫离子的测定,结果满意。     

Thermus thermophilus 木糖异构酶与木糖醇的分子对接及模型分析

在1BXB结构基础上, 通过分子对接方法构建木糖异构酶与抑制剂木糖醇的复合物模型, 为合理设计解除木糖醇对木糖异构酶的抑制及进一步揭示木糖醇对该酶抑制机理提供参考.     

固体电解质La2-xCaxMo1.7W0.3O9-δ(0≤x≤0.2)的合成、表征及电性能

在氧离子导体La₂Mo_1.7W_0.3O₉的基础上，采用固相法合成了La位掺杂的Ca系列新型氧化物La_2-xCa_xMo_1.7W_0.3O_9-δ(0≤x≤0.2)。通过XRD、Raman和XPS等手段对化合物结构进行表征，交流阻抗谱测试其电性能。结果表明：掺杂离子Ca²⁺的半径小于基质离子La³⁺的半径导致晶格收缩；Ca的掺杂在La₂Mo_1.7W_0.3O₉自身内置氧空位的基础上增加了额外的氧空位，提高了氧离子导体的电导率，550 ℃电导率由0.79 × 10^-4 S·cm^-1 (x=0.0)增加到1.5 × 10^-4 S·cm^-1 (x=0.16，0.2)，电导率增加89.9%。     

Study of Structures and Electronic Properties of Pdn–1Pb and Pdn （n≤8） Clusters

Geometric and electronic properties of Pdn–1Pb and Pdn (n≤8) clusters have been studied by using density functional theory with effective core potentials, focusing on the differences between mono- and bimetallic clusters. The average bond length of Pdn–1Pb (n≤8) bimetallic clusters is longer than that of pure palladium clusters except for n = 2 and 3. The most stable structure of Pdn–1Pb (n≤7) is the singlet where there is at least a Pd or Pb atom on its excited state. The energy gaps of Pd–Pb binary clusters are narrower than those of Pdn clusters, and then the chemical activity is strengthened when Pdn clusters are doped with Pb.     

不同形貌氧化镍纳米材料的合成及其电化学性能

以水-乙二醇为溶剂,以聚乙烯吡咯烷酮(PVP)为表面活性剂,采用溶剂热法合成了NiO纳米片,NiO纳米薄片通过自组装形成花状结构。 改变反应温度和溶剂,制备了NiO纳米立方体颗粒和NiO纳米球形颗粒。 用合成的NiO纳米材料制备工作电极,在6 mol/L的KOH溶液中利用三电极体系进行了电化学性能测试。 在电化学性能测试中进行了循环伏安测试、恒电流充放电测试和电化学阻抗谱(EIS)测试。 结果表明,NiO纳米片的比电容最高(在电流密度为0.5 A/g时比电容值为402 F/g),倍率性能最佳(0.5 A/g增加至4 A/g时有80.1%的电容保持率)。 在电流密度为4 A/g时对NiO纳米片进行1000次恒流充放电循环测试,比电容损失了9.7%。     

Lithium dioxobis[trioxoiodato(V)]vanadate,Li[VO2(IO3)2]

The title compound represents a new structure type, in which distorted VO₆ octa­hedra are bridged by iodate groups to form infinite two‐dimensional [VO₂(IO₃)₂]⁻ layers that are separated by octa­hedrally coordinated Li⁺ cations.     

Two Novel Antifungal Saponins from Tibetan Herbal Medicine Clematis tangutica

Antifungal assay-guided isolation of the ethanol extract of the aerial parts of Clematis tangutica yielded two novel triterpene saponins. Their structures were determined to be 3-O-α-L-arabinopyranosyl hederagenin 28-O-α-L-rhamnopyranosyl ester (1) and 3-O-β-D-glucopyranosyl-(1→4)-α-L-arabinopyranosyl hederagenin 28-O-α-L-rhamnopyranosyl ester (2) on the basis of spectral data and chemical reactions.