水相法合成二氯二甲茂钛与水杨酸类配合物

Ｃｐ2 ＴｉＣｌ2 具有很好的抗癌活性 ,已成为第三代抗癌药物[1 - 3] 。为了寻求活性更高的抗癌药物 ,探索抗癌机理 ,我们用 (ＭｅＣｐ) 2 ＴｉＣｌ2 、水杨酸或其衍生物 ,按水相法合成了甲茂钛的水杨酸类配合物。合成路线如下图所示 :其中 :Ⅰ为ｐＨ <4 ,Ｘ =Ｈ ,Ｙ =Ｈ的产物 ;Ⅱ为ｐＨ <4 ,Ｘ =Ｈ ,Ｙ =ＮＯ2 的产物 ;Ⅲ为ｐＨ >6 ,Ｘ =ＮＯ2 ,Ｙ =ＮＯ2 ,Ｚ =Ｏ的产物 ;Ⅳ为ｐＨ >6 ,Ｘ =Ｈ ,Ｙ =Ｈ ,Ｚ =Ｓ的产物。 (Ⅰ～Ⅳ为新化合物 )1　实验部分1 .1　仪器与试剂水杨酸、ＴｉＣｌ4,ＡＲ ;5 -硝基水杨酸、3,5 -二硝基水杨酸、5 -磺基…     

Novel Gel—like Process for Synthesizing Submicron LiaNi0.8Co0.2O2 Powders Used in Lithium Ion Batteries

A novel gel-like process has been developed for synthesizing LiaNi0.8Co0.2O2 powders,using citric acid as a chelating agent. This process improves the homogeneity of constituent cation and enhances their reactivity in the obtained precursor. The results of electrochemical test demonstrated that these materials exhibited excellent electrochemical properties. Its initial capacity reached 181.6 mAh/g and reversible efficiency at the first cycle is about 88.6%.     

2,5—二取代—1,3—4—恶二唑和N,N‘—二酰基肼化合物的合成与生物活性

合成了１８种新的对称与不对称的２，５－二取代－１，３，４－恶二唑及Ｎ，Ｎ“＇－Ｆ二酰基肼化物，用元素分析，红外光谱，核磁氢谱和质谱确定了其结构，并对它们的杀虫，抗菌活性进行了测试，发现了数个具有较强生物活性的化合物。     

New ent‐Abietanoids from Isodon rubescens

Six new ent‐abietane diterpenoids, rubescensins I–M ( 1 – 5 ) and P ( 6 ), along with two related acetonide derivatives ( 7 and 8 ), were isolated from Isodon rubescens. Their structures were elucidated by detailed spectroscopic analysis. Compound 5 is the first N‐containing diterpenoid from the genus Isodon, exhibiting notable cytotoxicity against human tumor K562 cells.     

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.