EuI2—RbI二元体系相图

用差热分析和Ｘ射线粉末衍射法研究了ＥｕＩ２－ＲｂＩ二元体系相图。表明该体系是一个有４个化合物生成的复杂低共熔体系，其中ＲｂＥｕ２Ｉ５和ＲｂＥｕＩ３为固液同组成化合物，Ｒｂ３ＥｕＩ５和Ｒｂ４ＥｕＩ６为固液异组成化合物。初步确定Ｒｂ３ＥｕＩ５为立方晶系：ａ＝１．０１２４（１）ｎｍ；Ｒｂ４ＥｕＩ６为四方晶系：ａ＝１．３７１９（５）ｎｍ，Ｃ＝０．６４５８（５）ｎｍ．     

EuI_2－RbI二元体系相图

用差热分析和Ｘ射线粉末衍射法研究了ＥｕＩ２－ＲｂＩ二元体系相图。表明该体系是一个有４个化合物（ＲｂＥｕ２Ｉ５，ＲｂＥｕＩ３，Ｒｂ３ＥｕＩ５，Ｒｂ４ＥｕＩ６）生成的复杂低共熔体系，其中ＲｂＥｕ２Ｉ５和ＲｂＥｕＩ３为固液同组成化合物，Ｒｂ３ＥｕＩ５和Ｒｂ４ＥｕＩ６为固液异组成化合物。初步确定Ｒｂ３ＥｕＩ５为立方晶系：ａ＝１．０１２４（１）ｎｍ；Ｒｂ４ＥｕＩ６为四方晶系：ａ＝１．３７１９（５）ｎｍ，ｃ＝０．６４５８（５）ｎｍ。     

氯代亚乙烯基双噁唑的合成、晶体结构及其电子光谱

由氯代丁烯二酰氯和α－氨基苯乙酮的盐酸盐经缩合、关环反应合成了标题化合物Ⅰ、Ⅱ．用元素分析、紫外光谱、红外光谱、质谱鉴定了其结构，并用Ｘ射线衍射法测定了Ⅰ的晶体结构，其空间群为Ｐ２１，晶胞参数α＝０．８４５０（２）ｎｍ，ｂ＝０．６９９４（１）ｎｍ，ｃ＝１．５４３２（５）ｎｍ，β＝１０２．３８（２）°，Ｚ＝２．由于在烯键碳原子上引入体积较大的氯原子，使Ⅰ和Ⅱ分子的平面性变差，其电子光谱相对于反式－１，２－双［２－５－苯基唑基）］乙烯（ＰＯＥＯＰ）有蓝移，且荧光量子产率明显下降。     

（Ce0.67Tb0.33）MgAl11O19和BaMgAl10O17：Eu^2＋荧光体的微波辐 …

用微波辐射法合成了（Ｃｅ０．６７Ｔｂ０．３３）ＭｇＡｌ１１Ｏ１９（Ｐ－Ｇ）和ＢａｍｇＡｌ１０Ｏ１７（Ｐ－Ｂ）两种荧光体，经Ｘ射线粉末衍射分析，其ｄ值和Ｉ／Ｉ０值与ＪＣＰＤＦ３６－７３和２６－１６３基本一致。计算得到Ｐ－Ｇ的晶胞参数ａ＝０．５５８２ｎｍ，ｃ＝２．１８８４ｎｍ；Ｐ－Ｂ的晶胞参数ａ＝０．５６１６ｎｍ，ｃ＝２．２６１４ｎｍ，测定了两种荧光体的激发光谱和发射光谱，Ｐ－Ｇ的色坐标ｘ＝０．３１６     

Y2O2S：Eu^3＋荧光体的微波热效应合成和发光性能

用微波热效应法合成Ｙ２Ｏ３Ｓ：Ｅｕ＾３＋粉晶荧光体，经Ｘ射线粉末衍射分析确证其为六方晶系，计算得到其晶胞参数ａ＝０．３７８５ｎｍ，ｃ＝０．６５９０ｎｍ。激发光谱峰呈宽带状，最大激发光谱峰λｅｘ＝２６１ｎｍ，最大发射光谱峰λｅｎ＝６２６ｎｍ，其次还有５９５、６１７和７０６ｎｍ，归属为Ｅｕ＾３＋离子的＾５Ｄ０－＾７ＦＪ特征发射。     

一种高灵敏度的小檗碱高效液相色谱分析方法

根据在卤代烃类溶剂中的小檗碱在紫外线的激发下可产生强烈的荧光这一特性,采用正相色谱－荧光检测的方法建立了小檗碱的高灵敏度检测方法。色谱柱为ＬｉｃｈｒｏｓｏｒｂＳＩ６０（５μ）２０ｃｍ×４．０ｍｍｉ．ｄ．。流动相为二氯甲烷－甲醇－二乙胺－冰醋酸（９０：９：０．４：０．５）。荧光检测波长Ｅｘ＝３６５ｎｍ,Ｅｍ＝５１０ｎｍ。方法的检测限为０．２ｎｇ（Ｓ／Ｎ≥２．５）,在０．２ｎｇ～２０ｎｇ范围内具有良好的线性关系。     

二次锂电池正极材料LixNi0.3Co0.7O2的XPS与XRD研究

结果表明，ＬｉｘＮｉ０．３Ｃｏ０．７Ｏ２具有六方晶系Ｒ３＾－ｍ空间群结构。当Ｘ－１，０．３１５时，其晶胞参数分别为ａ＝２．８２６ｎｍ，ｃ＝１４．１３０ｎｍ和ａ＝０．２８０８ｎｍ，ｃ＝１．４２５３ｎｍ；ＭＯ６（Ｍ＝Ｎｉ，Ｃｏ）八面体中Ｍ－Ｏ平均距离分别为０。１９４１ｎｍ和０．１９３３ｎｍ。ＸＰＳ分析结果表明ＬＩｘＮｉ０．３ＣＯ０．７Ｏ２表面存在Ｌｉ２Ｏ，同时探讨了其中过渡金属离子的３ｄ电子结构变化。     

二次锂电池正极材料Li_xNi_（0．3）Co_（0．7）O_2的XPS与XRD

结果表明，ＬｉｘＮｉ０．３Ｃｏ０．７Ｏ２具有六方晶系Ｒ３－ｍ空间群结构。当Ｘ＝１，０．３１５时，其晶胞参数分别为ａ＝２．８２６ｎｍ，ｃ＝１４．１３０ｎｍ和ａ＝０．２８０８ｎｍ，ｃ＝１．４２５３ｎｍ；ＭＯ６（Ｍ＝Ｎｉ，Ｃｏ）八面体中Ｍ－Ｏ平均距离分别为０．１９４１ｎｍ和０．１９３３ｎｍ。ＸＰＳ分析结果表明ＬＩｘＮｉ０．３ＣＯ０．７Ｏ２表面存在Ｌｉ２Ｏ，同时探讨了其中过渡金属离子的３ｄ电子结构变化。     

邻香兰素与邻氨基苯甲酸Schiff碱铜（Ⅱ）配合物的合成、晶体结构和热分解动力学

合成了邻香兰素（２－羟基－３－甲氧基苯甲醛）与邻氨基苯甲酸Ｓｃｈｉｆｆ碱铜（Ⅱ）配合物，测定了其晶体结构并研究了其热稳定性。晶体Ｃ_（３０）Ｈ_（２８）Ｃｕ_２Ｎ_２Ｏ_（１１）属正交晶系，空间群Ｐｃａｎ，晶胞参数：ａ＝１．０３４７（４）ｎｍ，ｂ＝１．５４９３（７）ｎｍ，ｃ＝１．７４４１（３）ｎｍ，Ｖ＝２．７９５９ｎｍ~３，Ｍ＝７１９．６４，Ｚ＝４。结构解析最终的一致性因子Ｒ＝０．０４７，Ｒｗ＝０．０４９，热分解反应动力学方程式为：ｄα／ｄｔ＝Ａ·ｅ~（－Ｅ／ＲＴ）·３（１－α）~（２／３）；其补偿效应数学表达式为：１ｎＡ＝０．２８５８Ｅ＋０．４０４５。     

高压后EuI2的结构及光谱性质研究

研究了高压后ＥｕＩ２的结构及光谱性质，发现高压后其结构由单斜转化为正交，对称性和Ｅｕ＾２＋配位数均有增加，４ｆ＾６５ｄ能级间距加大，能级重心降低。还讨论了发射光谱的红移现象，指认了新出现的４４９ｎｍ处的发射峰，并报道了ＥｕＩ２新的正交结构（ＥｕＩ２－Ｖ）。     

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%.     

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.     

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.     

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

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.     

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.