La0.8Ca0.2MnO3纳米线的制备及表征

利用Sol-gel法结合氧化铝模板技术制备了La0.8Ca0.2MnO3纳米线, 并研究了两种热处理方法对 La0.8Ca0.2MnO3纳米线结构和形貌的影响. 快速升温到800 ℃得到的La0.8Ca0.2MnO3纳米线较粗, 其直径大于氧化铝模板的孔径, 而经过缓慢升温到400 ℃预处理再升温到800 ℃得到的La0.8Ca0.2MnO3纳米线, 其直径和氧化铝模板的孔径相当, 都约为35 nm. X射线衍射和透射电镜分析结果表明, 两种方法得到的 La0.8Ca0.2MnO3纳米线都是具有钙钛矿结构的属于单斜晶系的多晶材料.     

双2-乙酰基二茂铁合汞的合成及其晶体结构

标题化合物(C24H22Fe2HgO2)3是由2 氯汞基 1 乙酰基二茂铁与乙二胺反应得到的,其结构通过单晶X 射线衍射法确定。其晶体属三斜晶系,P 1空间群,Mr=1964 12,a=10 193(2),b=11 504(2),c=14 413(3) ,α=92 21(3),β=104 12(3),γ=102 67(3)°,V=1591 55(5) 3,Z=1,Dc=2 049mg/cm3,μ=8 583mm-1,F(000)=942,最终偏离因子为R=0 0859,wR=0 2617。该晶体中同时含有meso型及dl型分子,各分子中Hg原子的配位情况不一样。meso分子中的两个二茂铁是相互平行的,而另两分子dl型的二茂铁是相互垂直的。Hg原子以桥联形式连接两个二茂铁部分。meso型与dl型分子通过Hg O弱配位作用相连。     

微波辐射下2-氨基-7-甲基-4-芳基-5-氧代-4H,5H-吡喃并[4,3-b]吡喃-3-腈的一步合成

芳醛、丙二腈与6-甲基-4-羟基-2-吡喃酮在微波辐射下, 一步反应得到一系列2-氨基-7-甲基-4-芳基-5-氧代-4H,5H-吡喃并[4,3-b]吡喃-3-腈, 该反应时间短、产率较高、环境友好、后处理简单. 产物的结构经红外光谱、核磁共振谱和元素分析表征, 产物4g的结构经单晶X射线衍射进一步确证; 并对反应过程提出了可能的机理.     

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.