二苯骈－21－冠－7与12－磷钨酸铯配合物的合成及表征

二苯骈－２１－冠－７与１２－磷钨酸铯配合物的合成及表征陈伟，罗良琼（四川联合大学（东区）化学系成都６１００６４）关键词合成，冠醚配合物，１２－磷钨酸铯二苯骈－２１－冠－７（ＤＢ２１Ｃ７）与含简单阴离子的铯盐配合物已有一些研究［１］，但是ＤＢ２１Ｃ７与...     

冠醚DPDB－18－C－6与钾显色反应的分光光度法研究

冠醚ＤＰＤＢ－１８－Ｃ－６与钾显色反应的分光光度法研究黄青瑜，营豫梅，谢明贵（四川联合大学化学系成都６１００６４）关键词钾，二苦胺基二苯并－１８－冠－６，分光光度法目前碱金属的光度测定，较为广泛的是借助阴离子染料生成三元配合物的显色方法［１－２］。近...     

2，3－二氰基－2，3－二（X－取代苯基）丁二酸二乙酯在苯乙烯中的分解动力学研究

２，３－二氰基－２，３－二（Ｘ－取代苯基）丁二酸二乙酯在苯乙烯中的分解动力学研究齐陈泽，吴靖嘉，段大勇，贾志胜，张斌，杨第伦（兰州大学应用有机化学国家重点实验室，兰州大学化学系，兰州，７３００００）关键词２，３－二氰基－２，３－二（Ｘ－取代苯基）丁二...     

2－氯／2－甲磺酰基－5－（2－苯基－4－喹啉基）－1，3，4－噁二唑化合物的合成及其亲核取代的研究

借处理２－羟基－５－（２－苯基－４－喹啉基）－１，３，二唑同ＰＣｌ＿５／ＰＯＣｌ＿３之间的反应合成了２－氯－５－（２－苯基－４－喹啉基）－１，３，４－二唑（３）和通过２－基－５－（２－苯基－４－喹啉基）－１，３，４－二唑的甲基化，然后氧化制得２－甲磺酰基－５－（２－苯基－４－喹啉基）－１，３，４－二唑（６）．并分别研究了３和６同胺、叠氮及肼的反应，得到２，５－二取代的二唑新衍生物．初步观察了部分化合物的抗菌活性．     

稀土元素荧光增强效应的研究──RE对Eu－2－（2－二苯乙酰基）－1，3－茚二酮－十六烷基三甲基溴化铵体系的荧光增强

研究了稀土元素Ｌａ~（３＋）、Ｇｄ~（３＋）、Ｙｂ~（３＋）、Ｌｕ~（３＋）、Ｙ~（３＋）及Ｓｃ~（３＋）对Ｅｕ－２－（２－二苯乙酰基）－１，３－茚二酮－阳离子表面活性剂体系的荧光增强效应，结果表明，在上述增强离子存在下，体系的荧光强度分别增加１０、１３０、３０、５０、５２和２０倍，利用标准加入法测定了混合稀土氧化物中的铕，铕浓度在１．０×１０~（－１０）～６．０×１０~（－７）ｍｏｌ／Ｌ范围内与荧光强度呈线性关系，最低检出限为６．０×１０~（－１２）ｍｏｌ／Ｌ。     

2－（1，3－亚丙二硫基）亚甲基环己酮的晶体结构

报导了标题化合物Ｃ_（１０）Ｈ_（１４）ＯＳ_２（Ｍ_ｒ＝２１４．３５）的晶体结构，该晶体属正交晶系，空间群为Ｐ２_１２_１２_１，晶胞参数为ａ＝６．４４３（３），ｂ＝８．９８０（４），ｃ＝１８．２１３（７）；Ｖ＝１０５３．８（６）３；Ｚ＝４，Ｄ_ｘ＝１．３５ｇ／ｃｍ~３，Ｆ（０００）＝４５５，μ＝４．５ｃｍ~（－１）（ＭｏＫａ）。最终偏离因子Ｒ＝０．０３３，Ｒ_ｗ＝０．０３４。分子中的两支Ｃ_（ｓｐ）２－Ｓ键键长近于相等，分别为１．７６１（３）和１．７６９（３），Ｃ（１）－Ｃ（５）键长为１．３６１（４）。     

2－（1，3－亚丙二硫基）亚甲基环己酮的晶体结构

报导了标题化合物Ｃ_（１０）Ｈ_（１４）ＯＳ_２（Ｍ_ｒ＝２１４．３５）的晶体结构，该晶体属正交晶系，空间群为Ｐ２_１２_１２_１，晶胞参数为ａ＝６．４４３（３），ｂ＝８．９８０（４），ｃ＝１８．２１３（７）；Ｖ＝１０５３．８（６）３；Ｚ＝４，Ｄ_ｘ＝１．３５ｇ／ｃｍ~３，Ｆ（０００）＝４５５，μ＝４．５ｃｍ~（－１）（ＭｏＫａ）。最终偏离因子Ｒ＝０．０３３，Ｒ_ｗ＝０．０３４。分子中的两支Ｃ_（ｓｐ）２－Ｓ键键长近于相等，分别为１．７６１（３）和１．７６９（３），Ｃ（１）－Ｃ（５）键长为１．３６１（４）。     

2－羟基2＇烷氧基－1，1＇－联萘化合物的~1HMNR研究

研究了２－羟基－２＇－异丙氧基－１。１－联萘（３）等联萘化合物的~１ＨＮＭＲ谱或ＣＯＳＹ谱。此类化合物因２及２＇位取代基不同，两个萘环上同位质子不再等价，萘环质子峰增至１２组。化合物３~１ＨＮＭＲ谱峰的归属表明，萘环环电流各向异性对另一萘环质子的屏蔽作用与作者早期研究结果［１］一致。２（或２＇）位取代基上的质子的化学位移也与另一萘环平面相对位置有关。     

氧化镁表面辐射接枝聚合反应机理研究

氧化镁表面辐射接枝聚合反应机理研究蒋波＊黄光琳（四川联合大学原子核科学技术研究所成都６１００６４）（四川联合大学化学系成都）关键词氧化镁，反应机理，辐射接枝，甲基丙烯酸甲酯１９９６－０５－２１收稿，１９９６－０８－２６修回辐射诱发有机单体在固体表面聚...     

6，6＇－二（二苯基氧化膦甲基）－1，1＇－氮氧化－2，2＇－联吡啶与硝酸铒配合物的合成与结构

合成了硝酸铒与四功能团含磷萃取剂６，６＇－二（二苯基氧化膦甲基）－１，１＇－氮氧化－２，２＇－联吡啶的配合物。用四圆衍射仪测定了配合物的晶体结构。晶体属单斜晶系，空间群Ｃ２／ｃ，晶体学参数，ａ＝１．９８３０（４）ｎｍ，ｂ＝２．３１３５（４）ｎｍ，ｃ＝１．８６００（３）ｎｍ；β＝９６．１８（２）°，ｚ＝４。配合物中有机配体以四齿形式与中心离子铒配位，金属离子的配位数为８。配位几何构形为稍变形的四方反棱柱。金属离子周围的配位水分子已全部被取代。     

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.     

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.     

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.     

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.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.