不同金属离子对Co/Al2O3中Co的分布和CoMoK/Al2O3催化活性的影响

在γ－Ａｌ２Ｏ３咖入Ｚｎ＾２＋，Ｍｇ＾２＋，Ｃｕ＾２＋或Ｃｒ＾３＋后用漫反射光谱法研究了它们对随后加入的Ｃｏ分布的影响，同时还研究了这些离子对水煤气变换反应催化剂ＣｏＭｏＫ／Ａｌ２Ｏ３的催化活性的影响，发现Ｚｎ＾２＋，Ｍｇ＾２＋具有阻止Ｃｏ进入载体内层的作用，Ｃｕ＾２＋，Ｃｒ＾３＋的作用则相反，四面体配位倾向强的金属离子能阻Ｃｏ进入载体内层，从而促进水煤气变换反应的催化活性，而八面配位倾向强度金属     

玉米素和激动素的伏安行为

玉米素和激动素在０．１ｍｏｌ／Ｌ的醋酸－醋酸钠底液里能还原，产生很好的极谱峰，检测灵敏度可达２．５×１０＾－＾８ｍｏｌ／Ｌ，峰电位分别为－１．１８Ｖ和－１．１７Ｖ（对Ａｇ／ＡｇＣｌ）。测定了电极反应决定步骤的αｎα和电化学反应的标准速率常数ｋｓ，研究了它们对Ｃｕ＾２＾＋，Ｅｕ＾３＾＋，Ｃｄ＾２＾＋，Ｚｎ＾２＾＋的电极不产生的影响。     

Eu^2＋和Mn^2＋在Sr3MgSi2O8中的光致发光研究

研究了Ｅｕ＾２＋和Ｍｎ＾２＋共激活的Ｓｒ３ＭｇＳｉ２Ｏ８的荧光性质。Ｅｕ＾２＋和Ｍｎ＾２＋在４６０ｎｍ和６９０ｎｍ的发射峰分别由Ｅｕ＾２＋的５ｄ→４ｆ跃迁和Ｍｎ＾２＋的＾４Ｔ１（＾４Ｇ）→＾６Ａ１ｇ（＾６Ｓ）跃迁产生。未观察到单掺杂Ｍｎ＾２＋的Ｓｒ３ＭｇＳｉ２Ｏ８的荧光发射，而掺入Ｅｕ＾２＋后则出现了Ｍｎ＾２＋的６９０ｎｍ光致发光峰，表明Ｅｕ＾２＋对Ｍｎ＾２＋有敏化作用。Ｅｕ＾２＋的荧光寿命也受Ｍ     

利用葡萄糖氧化酶反应体系动力学光度法测定痕量银

基于葡萄糖氧化酶－过氧化物酶－４－氨基安替比林－２，４－二氯苯酚偶联反应的动力学性质及Ａｇ＾＋，Ｈｇ＾２＋，Ａｌ＾３＋，Ｃｕ６２＋等离子对反应的影响，建立了用动力学光度法测定痕量银的新方法。     

PTFE—乙醚柱反相萃取层析连续分离和测定镓（Ⅲ）铟（Ⅲ）的研究

研究了在抗坏血酸存在下的６ｍｏｌ／Ｌ ＨＢｒ介质作流动相，以ＰＴＦＥ（聚四氟乙烯）负载的乙醚作固定相，反相萃取层析使微量Ｇａ（Ⅲ），Ｉｎ（Ⅲ）与Ｆｅ＾３＋、Ｔｌ＾３＋、Ｍｏ＾６＋、Ａｕ＾３＋、Ｔｉ＾４＋、Ｂｉ＾３＋、Ａｌ＾３＋、Ｍｇ＾２＋、Ｃａ＾２＋、Ｎｉ＾２＋、Ｃｏ＾２＋、Ｃｄ＾２＋、Ｚｎ＾２＋、Ｐｂ＾２＋、Ｃｕ＾２＋等多种离子分离。留于柱上的铟、镓分别用ＨＣｌ（４ｍｏｌ／Ｌ）－Ｈ２Ｏ２（３％）     

Eu2+在多相体系中的发光

研究了基质结构与离子半径的形成关系和Ｅｕ２＋在同时形成的多相体系中的发光现象．在ＭＭｇＡｌ１０Ｏ１７体系中,当Ｍ离子半径小于０．１０ｎｍ时,体系形成多相共存．首次观察到在磁铅矿、尖晶石和α－Ａｌ２Ｏ３三相同时共存体系中,Ｅｕ２＋优先占据离子半径和电荷与之匹配的磁铅矿中的Ｃａ２＋离子格位,不进入尖晶石和α－Ａｌ２Ｏ３晶相中的Ｍｇ２＋、Ａｌ３＋离子格位,仅产生Ｅｕ２＋的ｄ→ｆ跃迁宽带发射,且观察不到Ｅｕ３＋的特征光谱;在尖晶石和α－Ａｌ２Ｏ３两相同时共存体系中,Ｅｕ２＋可进入尖晶石和α－Ａｌ２Ｏ３晶相中的Ｍｇ２＋、Ａｌ３＋离子格位,分别产生Ｅｕ２＋的ｄ→ｆ和ｆ→ｆ跃迁发射,同时还观察到相当强的Ｅｕ３＋的特征光谱;在α－Ａｌ２Ｏ３单一相中,Ｅｕ２＋产生ｆ→ｆ跃迁发射,并观察到明显的Ｅｕ３＋的特征光谱,在α－Ａｌ２Ｏ３与γ－Ａｌ２Ｏ３同时存在的混合相中,Ｅｕ２＋的ｆ→ｆ跃迁发射消失,产生新的ｄ→ｆ跃迁宽带发射     

ICP—AES间接法连续测定混合物中的氯和碘离子的研究

本文研究了在Ｃｌ和Ｉ＾－的混合物中，加入过量Ａｇ＾＋使Ｃｌ＾－和Ｉ＾－分别以ＡｇＣｌ和ＡｇＩ沉淀后，用ＩＣＰ－ＡＥＳ测定剩余的Ａｇ＾＋，然后用ＮＨ３．Ｈ２Ｏ溶解ＡｇＣｌ沉淀，测定溶解液中的Ａｇ＾＋，间接得到Ｃｌ＾－的含量，以差减法求得Ｉ＾－量，实现Ｃｌ＾－和Ｉ＾＿的间接法连续测定。本文探讨了有关的化学条件和光谱测定条件，对方法的适用性进行了考察－共存离子的干扰情况，方法的精密度，检出限和试样中加入     

新试剂N—烯丙基—N‘—（氧基对苯磺酸钠）硫脲（ASATu）的合成,表征及其反…

本文报道了新试剂Ｎ－烯丙基－Ｎ＇－（氨基对苯磺酸钠）硫脲（ＡＳＡＴｕ）的合成并确定了结构。该试剂与４５种元素在不同介质中反应，仅有Ｃｕ＾２＋，Ａｇ＾＋，Ｂｉ＾３＋，Ｈｇ＾２＋和Ｆｅ＾３＋等离子产生特征性反应。实验证明，它可作为Ｃｕ＾２＋，Ａｇ＾＋等新的鉴定试剂；在酸性和近中性介质中测定了该试剂与稀土元素等四十多种金属元素反应的摩尔吸光系数。     

不同金属离子对CO／Al_2O_3中Co的分布和CoMoK／Al_2O_3催化

在γ－Ａｌ２Ｏ３中加入Ｚｎ２＋，Ｍｇ２＋，Ｃｕ２＋或Ｃｒ３＋后用漫反射光谱法研究了它们对随后加人的Ｃｏ分布的影响，同时还研究了这些离子对水煤气变换反应催化剂ＣｏＭｏＫ／Ａｌ２Ｏ３的催化活性的影响．发现Ｚｎ２＋，Ｍｇ２＋具有阻止Ｃｏ进入载体内层的作用，Ｃｕ２＋，Ｃｒ３＋的作用则相反．四面体配位倾向强的金属离子能阻止Ｃｏ进入载体内层，从而促进水煤气变换反应的催化活性，而八面体配位倾向强的金属离子的效果刚好相反．在６５０℃下，１００ｇＡｌ２Ｏ３含７ｇＭｇＯ时，Ｍｇ能最大限度地阻止Ｃｏ向Ａｌ２Ｏ３内层扩散，从而提高了ＣｏＭｏｋ／Ａｌ２Ｏ３的催化活性．     

一阶导数吸光光度法同时测定纯硅中铁和铝的研究

提出了用一阶导数光光度法同时测定铁和铝的方法，在ｐＨ６．５乙二胺缓冲溶液中，乳化剂ＯＰ存在下，Ｆｅ＾３＋Ａｌ＾３＋与络天青Ｓ形成Ｆｅ＾３＋，Ａｌ＾３＋－ＣＡＳ－ＯＰ三元络合物，络合物一阶导数光谱等吸收点分别在６０６．２，６３８．０ｎｍ记录混合体系在两波长处一阶导数数值可以分别测定铝，铁含量，互不影响，铁，铝含量分别在１．０～１６μｇ／２５ｍｌ，０．３～１０μｇ／２５ｍｌ范围内呈良好线性，用于测定纯     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.