Silica-supported Copper（Ⅱ） Catalyzed Coupling of Arylboronic Acids with Imidazoles

Immobilized copper（Ⅱ） in organic-inorganic hybrid materials catalyzed Ar-N coupling of arylboronic acids with imidazoles has been developed. Arylboronic acids reacted with imidazoles smoothly in the presence of a 3-（2-aminoethylamino）propyl functionalized silica gel immobilized copper（Ⅱ） catalyst （10 mol%） in methanol without any additives and bases. The reactions generated the corresponding cross-coupling products in good yields. Furthermore, silica-supported copper can be recovered and recycled by a simple filtration procedure and used for five consecutive trials without decreases in activity.     

Synthesis, Structure and Biological Activities of 2-Methylthio-3-cyano-7-（4-methoxyphenyl）- pyrazolo[1,5-a]pyrimidine

1INTRODUCTION Pyrazolo[1,5-a]pyrimidine derivatives have shown various biological activities in the terms of antibac-terial,antischistosomal and xanthine oxidase inhibi-tors[1~5].The enaminones are highly reactive inter-mediates and have been extensively used as build-ing blocks in organic synthesis especially in the he-terocyclic compounds[6~8].In addition,a great deal of interest has been focused on the synthesis of py-razolo[1,5-a]pyrimidine through versatile enamino-nes because of thei…     

稀土乙酰丙氨酸咪唑配合物的合成及光谱性质

稀土元素由于特殊的外层电子构型,在与不同类型配体配位时,呈现出丰富多彩的配位行为和结构,其配合物,特别是有机配合物,由于具有发光性强、选择性好的特点,在发光、激光材料创制、结构探针、荧光免疫分析及生物传感器等领域的研究和应用引起广泛关注.氨基酸、肽是各种生物大分子的基本组成单元,咪唑存在于组氨酸、羧肽酶、血红蛋白等生物分子中参与配位或"变构效应"成为活性部位结构,唑环有丰富的能级,其作为含N富电子体系可与稀土离子形成既有生物活性,又有优良光学性能的配合物.     

一种卟啉结构硫离子荧光探针的合成及荧光性能

以卟啉为荧光发色团,4-氯-7-硝基苯并-2-氧杂-1,3-二唑为识别基团,设计合成了一种具有较高选择性、高灵敏度的近红外硫离子荧光探针,其结构经~1H NMR,IR和HR-MS(ESI)表征。该合成路线简短,后处理简单。以荧光光谱为检测手段,测试了该探针分子对硫离子的识别效果。结果表明,此探针不仅具有高选择性和灵敏度,且在1. 0×10~(-6)～7. 0×10~(-6)mol·L~(-1)的浓度范围内呈现良好的线性关系,其检出限为78 nm。     

Partial Oxidation of Methane to Synthesis Gas over Hexaaluminates LaMAl11O19-δ catalysts

A series of M-substituted hexaaluminates LaMAl11O19-δ (M=Fe, Co, Ni, Mn, and Cu)were prepared and characterized by XRD, XPS, TPR and TGA techniques, respectively. They exhibited different reducibility and catalytic activity for partial oxidation of methane (POM) to synthesis gas. Among the LaMAl11O19-δ samples, LaNiAl11O19-δ showed the best catalytic activity for the topic reaction and selectivity for synthesis gas at 780 ℃ for 2 h. The conversion of CH4 was over 99.2%, and the product selectivity for both CO and H2 was above 90.3%.     

水中氯苯类污染物的顶空液相微萃取 GC-MS法测定

研究了用顶空液相微萃取GC-MS法测定水中的痕量氯苯类有机污染物。通过实验选择正辛醇为萃取剂,考察了萃取剂的体积、萃取温度、萃取时间、搅拌速度、样品顶空体积以及盐效应等对萃取的影响。在最佳萃取和测定条件下,方法的线性范围为0.1~800μg/L,检出限(S/N=3)为0.05~0.1μg/L。用本方法测定了实际样品及回收率,结果满意。     

μ-氧-双[三(对氟苄基)锡]的合成、表征及晶体结构

The μ-oxygen-bis[tri(p-fluorobenzyl)tin] was synthesized. The structure were characterized by elementary analysis, IR and ¹H NMR and the crystal structure were determined by X-ray single crystal diffraction. The crystal of the title compound belongs to rhombohedral with space group R, a=1.346 4(4), b=1.346 4(4), c=1.772 9(7) nm, α=90°, β=90°, γ=120°, Z=3, V=2.783 2(15) nm³, D_c=1.625 g·cm^-3, μ(Mo Kα)=1.408 mm^-1, S=1.088, F(000)=1 350, R₁=0.027 5, wR₂=0.065 9. In compound, the tin atom has a distorted tetrahedral coordination configuration. CCDC: 257079.     

红色长余辉发光材料Ca2Zn4Ti15O36：Pr^3＋的合成和发光性质

分别采用高温固相法和溶胶-凝胶法合成了新型红色长余辉发光材料Ca2Zn4Ti15O36:Pr。高温固相法合成Ca2Zn4Ti15O36需要在1200℃灼96h才能形成纯物相。热重分析曲线和X射线衍射分析结果表明：溶胶-凝胶法制得的前驱体在700℃灼烧12h开始形成Ca2Zn4Ti15O36物相；在1000℃灼烧24h得到Ca2ZnTi15O36纯物相；最佳反应温度为1000℃，激活剂Pr^3 的最佳浓度为0．6mol％，发光强度比高温固相法增强了510％。     

流动注射-原子吸收法间接测定扑尔敏

扑尔敏(马来酸氯苯那敏)是一种最常用的抗组织胺类药物。对其含量的测定，药典法采用非水滴定法和紫外分光光度法，此外还有分光光度法、电化学方法、高效液相色谱法以及ICP发射光谱间接测定法。这些方法均存在操作步骤繁琐的缺点。雷氏盐在酸性介质中可与大部分的有机碱(胺类、季铵盐类、含氮杂环类、生物碱类)等药物定量反应，生成难溶于水的络合物，故可以进行这些药物的鉴别、分离和含量测定。采用流动注射方法在线快速分离原子吸收法测定     

聚(Nε-苄氧羰基赖氨酸)-聚乙二醇-聚(Nε-苄氧羰基赖氨酸)的合成及其表征

利用三光气合成了Nε-苄氧羰基赖氨酸酸酐(Lys(z)-NCA),并用双端氨基聚乙二醇做引发剂,在DMF中引发Lys(z)-NCA聚合,合成了聚(Nε-苄氧羰基赖氨酸)-聚乙二醇-聚(Nε-苄氧羰基赖氨酸)三嵌段共聚物.利用IR、1H NMR、DSC和GPC对其结构进行了表征,结果表明,这种方法能够合成分子量可控、分子量分布窄(Ip=1.06)的嵌段共聚物,产率95.4%.