藏药香芸火绒草Leontopodium Haplophylloides化学成分的研究

从藏药香芸火绒草Leontopodium Haplophylloides Hand Mazz的甲醇提取物中分得四个B环未取代的黄酮, 分别为乔松素(1), 高良姜素(2), 3, 7-二羟基-5-甲氧基黄(3), 3, 5-二羟基-7-甲氧基黄酮(4), 化合物(2)对人皮肤痤疮菌具有一定的疗效。     

The Chemical Speciation and Behavior of Mercury and Selenium in the Insoluble Fraction of Striped Dolphin Liver

Most of the mercury and selenium exist in the insoluble fraction of dolphin liver. After the insoluble fraction was digested by alkaline protease in the presence of 1% SDS, approximately 50% of Hg and Se consisted in the supernatant and the others in the residue. Gel filtration chromatography of the hydrolysate showed that 96% of Hg and 87% of Se were combined with the high molecular weight proteins stably, which cannot be substituted by the complex reagents.Mercury and selenium in the residue were confirmed as HgSe crystal.     

蛋氨酸合成酶催化反应研究Ⅴ：5-氨基-6-（3-羟基-4-溴丁基）尿嘧啶的合成研究

报导了5-氨基-6-（3-丁烯基）尿嘧啶、5-氨基-6-（3-羟基-4-溴丁基）尿嘧 啶的合成方法。以γ-取代的β-酮脂和O-甲基异尿硫酸盐为超始物，经6-取代尿嘧 啶（3）、6-取代-5-偶氮尿嘧啶（4）和未见文献报道的中间体6，首次合成了5-氨 基-6-（3-丁烯基）尿嘧啶（5）及5-氨基-6-（3-羟基-4-溴丁基）尿嘧啶（7）。     

制备条件对CdWO4纳米棒的光致发光性能的影响

以Na₂WO₄和CdCl₂为主要原料，在130 ℃水热制备了CdWO₄纳米棒，并用扫描电镜(SEM)、透射电镜(TEM)、粉末X射线衍射(XRD)和能谱元素分析(EDS)对产物进行了表征。结果表明，产物为长约100 nm，直径10～30 nm的CdWO₄纳米棒。研究了不同反应条件下制备的CdWO₄纳米棒的光致发光性能。     

Novel silver-containing supramolecular frameworks constructed by combination of coordination bonds and supramolecular interactions

The hydrothermal reactions of AgNO(3), 4,4'-bipy, and carboxylate ligands gave rise to three supramolecular architectures, namely [Ag(bipy)].H(2)SIPA.1/2bipy.H(2)O (1), [Ag(bipy)].1/2H(2)btec.H(2)O (2), and [Ag(bipy)](2).H(2)dpstc.2H(2)O (3) (H(3)SIPA = 5-sulfoisophthalic acid, bipy = 4,4'-bipyridine, H(4)btec = 1,2,4,5-benzenetetracarboxylic acid, H(4)dpstc = 3,3',4,4'-tetracarboxydiphenyl sulfone). All complexes are extended from Ag-bipy linear chains by the combination of coordination bonds and supramolecular interactions in two different approaches. Complexes 1 and 3 comprise two-dimensional frameworks. In the two complexes, a one-dimensional ladderlike structure is first formed by the connection of a Ag-bipy chain through hydrogen bonding between a free carboxylate/bipy ligand and weak coordinative interactions between a free carboxylate ligand and silver ion. The ladderlike structure is then extended to a two-dimensional layer architecture by pi...pi interactions between bipy ligands of the Ag-bipy chains. Complex 2 possesses a three-dimensional framework. The free H(2)btec(2)(-) ligands form a two-dimensional layer network by hydrogen-bonding interactions between protonated and deprotonated carboxylate groups; meanwhile, pi.pi interactions between bipy ligands of Ag-bipy chains also result in a two-dimensional layer. The two layers are further connected by weak Ag-O interactions to generate a three-dimensional supramolecular structure.     

Chiral Phosphinophenyloxazolines Bearing Alkoxymethyl Substituents: Synthesis and Application in the Palladium Catalyzed Allylic Substitution Reactions

The chiral phosphine‐oxazoline ligands 3 and 4 bearing 4‐alkoxymethyl substituents on the oxazoline ring with (R)‐configuration were prepared from L‐serine methyl ester in 66% and 33% yields, respectively. Along this synthetic pathway, the β‐hydroxylamides derived from L‐serine methyl ester and 2‐halobenzoyl chlorides were expediently converted to the corresponding oxazolines by using diethylaminosulfur trifluoride as the activation agent. Potassium diphenylphosphide was the reagent of choice for replacing the bromine atom on the phenyl ring, giving the desired oxazoline‐phosphine ligands 3 and 4 . Together with [Pd(η³‐allyl)Cl]₂, ligands 3 and 4 induced an enantioselective allylic substitution reaction of 1,3‐diphenyl‐2‐pro‐penyl acetate by dimethyl malonate. Although ligands 3 and 4 exhibit the (R)‐configuration, differing from the (S)‐configuration of Pfaltz‐Helmchen‐Williams phosphine‐oxazoline ligands, all these ligands led to the same enantiotopic preference in the allylic substitution reaction. To facilitate the recovery and reuse of the phosphine‐oxazoline ligand, immobilization on Merrifield resin was attempted, albeit in low loading.     

催化动力学光度法测定微量钯

在硫酸 ( 1 + 1 )介质中 ,Pd(Ⅱ )催化过氧化氢氧化酸性铬蓝K的褪色反应。研究了反应的最佳条件 ,建立了催化光度法测定痕量钯的新方法。方法的最低检测限为 5 97× 1 0 - 4 μg/mL。线性范围为 5 97× 1 0 - 4 ～ 2 60× 1 0 - 2 μg/mL。该法用于合成样品和含钯催化剂的分析     

Preparation and properties of polymer and quantum dot composites

Quantum dots (QDs) were prepared in an organic system through a simple and low-cost wet chemistry method. Polymer beads with a diameter of 60–70 nm and specific functional groups were synthesized by a particular seeded emulsion polymerization technique. QDs were embedded in the polymer beads with the specific functional groups through dissolving and swelling method, which provided the condition for the conjunction of biomolecules and QDs as fluorescent probes. The prepared composites were characterized with UV-Vis, PL, TEM, FTIR, CLSM and conductance titration etc. The results show that QDs are successfully embedded in polymer beads, which breaks the limitation that the conjunction of biomolecules and QDs can be achieved only for those synthesized in aqueous system. __________ Translated from Journal of Shanghai Jiaotong University, 2005, 39(1) (in Chinese)     

COMPUTER SIMULATION OF A SINGLE POLYMER CHAIN IN DIFFERENT SOLVENTS

In the present paper, the behavior of a single polymer chain under various solvent conditions was modeled by self-avoiding walks (SAW) with nearest neighbors attraction Δε on a simple cubic lattice. Determination of the θ-condition wasbased on the numerical results of the mean square radius of gyration and end-to-end distance. It was found that at the θtemperatue Δε/kT equals -0.27. The exponents a in the Mark-Houwink equation with different interaction parameters areconsistent with the results of experiments: under θ-condition, a = 0.5, and for a good solvent α= 0.74-0.84, respectively.     

双显色剂高灵敏协同显色反应的研究——钴(Ⅲ)-亚硝基R盐-结晶紫体系

在水溶液中钴(Ⅱ)与亚硝基R盐所形成的配合阴离子可以与有机碱阳离子(结晶紫)缔合形成中性缔合分子。在聚乙烯醇存在下,配合物可稳定存在于水溶液中。钴(Ⅲ)-亚硝基R盐-结晶紫配合物在510nm处有一最大吸收,摩尔吸光系数ε_(510)=1.47×l0~5L·mol~(-1)·cm(-1)。配合物中各组分的摩尔比为:Co:R:CV=1:3:6。反应具有较高的选择性,采用双峰双波长法测定钴可使灵敏度得到进一步提高,相应的摩尔吸光系数ε_(510-640)=4.09×10~5L·mol~(-1)·cm~(-1)。方法用于合成试样中钴的测定,结果满意。