Rh-Catalyzed Kinetic Resolution-Based Enantioselective [4+2]-Cycloaddition-Isomerization of Allene-1,3-dienes

The first example of Rh-catalyzed kinetic resolution of 1,3-disubstituted allene-1,3-dienes involving intramolecular[4+2]-cycloaddition has been developed.Follo...     

拉曼光谱在固相有机合成中的应用

本文综述了近几年以来拉曼光谱在固相有机合成中的应用研究进展,分别介绍了近红外傅立叶变换和共焦显微两种拉曼光谱技术。近红外傅立叶变换拉曼光谱克服了荧光背景带来的干扰,可以用在固载试剂、催化剂的表征、固相有机反应的监测等方面,特别对于在无机载体上进行的有机反应的表征和检测方面具有很大的优势。共焦显微拉曼光谱具有特殊的空间分辨能力,适合对固相合成载体的结构进行表征,并可对载体内部反应活性位点的分布情况进行研究。     

气相色谱-质谱法分析木奶果挥发油的化学成分

采用水蒸汽蒸馏法从大戟科木奶果中提取挥发油,用气相色谱-质谱对挥发油的化学成分进行了分析。鉴定出19种化合物,占总油量的100%,用面积归一化法测定了各成分的相对百分含量。木奶果挥发油主要成分为正十六碳酸、丁基甲氧基苯、9,12-十八碳二烯酸,分别占挥发油总量的29.53%、17.47%和11.59%,三者占其总量的58.59%。     

Crystal structure and thermal stability of A μ1,1-(OMe)-bridged dimeric Schiff base iron(III) complex

A new μ_1,1-OMe-bridged dimeric iron(III) complex, [Fe₂L₂(μ_1,1-OMe)₂(NCS)₂], where L is the deprotonated form of 2-[(2-ethylaminoethylimino)methyl]-5-methoxyphenol, has been prepared and structural characterized by elemental analysis, IR spectrum, and single crystal X-ray crystallography. The complex crystallizes in the monoclinic space group P2₁/c, with unit cell dimensions a = 10.156(1) Å, b = 11.972(1) Å, c = 14.256(2) Å, β = 102.643(3)°, V = 1691.3(3) ų, Z = 2, R ₁ = 0.0394, and wR ₂ = 0.0922. Each Fe atom in the complex is in an octahedral coordination. The Fe...Fe distance is 3.102(1) Å. The thermal stability of the complex was studied.     

Synthesis of a Nine-atom Germanium Cluster K_(0.5)[K(18-crown-6)]_(1.5)Ge_9·1.5en with Unprecedented “up” and “down” Chain Arrangement of Unit [-(Ge_9-K-Ge_9)~(3-)-]

A new complex K0.5[K(18-crown-6)]1.5Ge9·1.5en(1) which contains unprecedented "up" and "down" chain arrangement of unit [-(Ge-9-K-Ge9)3-] has been prepared by the reaction of K4Ge9 with HgS in ethylenediamine(en) in the presence of 18-crown-6(1,4,7,10,13,16-hexaoxacyclooctadecane), and characterized by X-ray structure analysis. The color of the title crystals(black), which is darker than that of the reported three compounds with chains of germanium clusters, may result from the naked K+ and their interactions with the chain. And the structure differences between 1 and the reported three compounds with chains of germanium have also been discussed.     

水介质中ATRP法制备PDMAEMA及其温敏性

在30℃下以溴化亚铜-溴化铜混合物为催化剂,五甲基二乙烯三胺(PMDETA)为配体,在水介质中利用原子转移自由基聚合法(ATRP)合成聚合度达到300的聚甲基丙烯酸N,N-二甲基氨基乙酯(PDMAEMA)。核磁共振结果显示,聚合反应符合一级反应动力学描述。利用紫外可见分光光度计(UV-Vis)表征该聚合物的温敏性,结果表明,随着PDMAEMA聚合物链长的增加,其最低临界溶解温度(LCST)可降低至31.4℃。     

Two 2D uranyl coordination complexes showing effective photocatalytic degradation of Rhodamine B and mechanism study

Two new hydrostable two-dimensional(2 D) uranyl coordination complexes [(UO_2)_5(μ_3-O)_2(nbca)_2].7 H_2O(1) and [(UO_2)_3(nbca)_2(H_2O)_3]·2 H_2O(2)(H_3 nbca=5-nitro-1,2,3-benzenetricarboxylic acid) were hydrothermal synthesized.Single-crystal structural refinements reveal that both of the two complexes were formed by the packing of 2D uranyl coordination sheets via the hydrogen bonds.The nbca ligand coordinating to the uranyl polyhedron centers constructed the 2D sheets.There are UO_8 hexagonal bipyramids and UO_7 pentagonal bipyramids in 1 while only U07 pentagonal bipyramids in 2.Photocatalytic degradation of rhodamine B(RhB) in aqueous solution was studied.Complex 2 possesses better performance than 1 with 96.2 % of the RhB was degraded in only 60 min.Mechanism studies reveal that the dissolved oxygens are essential to the RhB degradation.The photocurrent density of 2 is more stable than that of 1,which indicating the stronger ability to separate photoexcited electrons and hole pairs of 2.     

原子荧光光谱法直接测定二甲基二硒

硒位于第六主族,为准金属元素。在自然界中硒的存在形式按其结合形态分为无机硒和有机硒[1,2]。有机硒较无机硒具有更高的生物活性,因此准确测定各种样品中的有机硒具有重要意义。对于挥发性有机硒,一般采用洗脱富集将其与样品基体分离,采用固相吸附[3,4]或液氮冷阱捕集[5,6],热解析或溶剂萃取后用气相色谱测定[7,8]。这些方法可以提供许多有机硒的信息,但其不足之处是程序较为繁琐。原子荧光光谱分析法(AFS)具有准确度高、灵敏度高、线性范围宽、干扰少等优点,故本文利用AFS的特点及二甲基二硒(DMDSe)的挥发性,在不加任何试剂的条件下,…     

Relationships among Preparative Technique,Phase Composition and Bending Strength of Bauxite Porcelain

1 INTRODUCTION Bauxite porcelain is a novel “K2O–Al2O3–SiO2” system ceramic by using sintered bauxite, clay and potash feldspar and albite as the main raw materials with the Al2O3’s content of 50%～60(massfraction). Compared to the traditional“K2O–Al2O3–SiO2” feldspar porcelain by using quartz, bolus alb and potash feldspar and albite as the main raw materials, the bauxite porcelain possesses such advantages as high mechanical strength, excellent electrical insula- tion prop…