A Versatile Approach for the Asymmetric Synthesis of 3-Alkyl-isoindolin-1-ones

3 Ｓｕｂｓｔｉｔｕｔｅｄｉｓｏｉｎｄｏｌｉｎ 1 ｏｎｅｓ (2 ,3 ｄｉｈｙｄｒｏ 1Ｈ ｉｓｏｉｎｄｏｌｉｎ 1 ｏｎｅｓ)ｏｆｇｅｎｅｒａｌｓｔｒｕｃｔｕｒｅ (1)ｃｏｎｓｔｉｔｕｔｅｔｈｅｋｅｙｓｔｒｕｃｔｕｒａｌｆｅａｔｕｒｅｏｆａｌａｒｇｅｎｕｍｂｅｒｏｆｂｉｏａｃｔｉｖｅｍｏｌｅｃｕｌｅｓｏｆｎａｔｕｒａｌｏｒｓｙｎｔｈｅｔｉｃｏｒｉｇｉｎ .Ｆｏｒｅｘａｍｐｌｅ ,ｌｅｎｎｏｘａｍｉｎｅ (2 ) ,1ｎｕｅｖａｍｉｎｅａｎｄｃｈｉｌｅｎｉｎｅａｒｅａｌｋａｌｏｉｄｓｉｓｏｌａｔｅｄｆｒｏｍｖａｒｉｏｕｓ…     

A Facile Synthesis of Indolizines by 1，3－Dipolar Cycloaddition of Pyridinium and Related Heteroaromatic Ylides with Alkenes in the Presence of TPCD，Py_4Co（HCrO_4）_2

ＡＦａｃｉｌｅＳｙｎｔｈｅｓｉｓｏｆｉｎｄｏｌｉｚｉｎｅｓｂｙ１，３－ＤｉｐｏｌａｒＣｙｃｌｏａｄｄｉｔｉｏｎｏｆＰｙｒｉｄｉｎｉｕｍａｎｄＲｅｌａｔｅｄＨｅｔｅｒｏａｒｏｍａｔｉｃＹｌｉｄｅｓｗｉｔｈＡｌｋｅｎｅｓｉｎｔｈｅＰｒｅｓｅｎｃｅｏｆＴＰ...     

A new Far-Infrared Fourier Spectrometer

Summary This article describes a new commercial Far-Infrared Fourier Spectrometer system which has been developed for routine spectroscopy in the 10–1000 cm^–1 spectral region. The instrument incorporates real-time data processing and has been automated wherever possible for foolproof operation. A versatile sample chamber allows a wide range of spectroscopic studies to be performed, on solids, liquids and gases over a wide range of temperatures. A number of spectra are presented to illustrate the performance and typical applications of this Fourier spectrometer.

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Ein neues fourier-spektrometer für das ferne infrarot

Zusammenfassung Nach einer kurzen Einführung in die Methode der Fourier-Spektroskopie wird ein neues kommerzielles Fern-Infrarot-Fourier-Spektrometer mit real-time Datenverarbeitungsanlage beschrieben. Das Gerät ist für die Spektroskopie im Bereich 10–1000 cm^–1 konstruiert und weitgehend automatisiert. Eine vielseitig verwendbare Probenkammer ermöglicht umfangreiche spektroskopische Untersuchungen von Festkörpern, Flüssigkeiten und Gasen in einem sehr großen Temperaturbereich. Anhand einer Reihe von Spektren werden Leistung und typische Anwendungen dieses Fourier-Spektrometers erläutert.

Lecture presented at Euroanalysis I Conference, 28. 8.–1. 9. 1972 in Heidelberg, Germany.     

Synthesis and Structural Characterization of a New Hydrogen-bonded Polyrotaxane of [Co(H2O)6]2+ with 1,1''-(Propane-1,3-diyl)dipyridinium-4-carboxylate

A new double betaine 1,1 '-(propane-1,3-diyl)dipyridinium-4-carboxylate L has been synthesized. Reaction of 1,1'-(propane-1,3-diyl)dipyridinium-4-carboxylate tetrahydrate 1 With Co(ClO4)2·6H2O leads to the formation of a new Co(Ⅱ) coordination compound,namely [Co(H2O)6]·2H2O·2L·2ClO4 2.The crystal structures of 1 and 2 have been determined by single-crystal X-ray diffraction method. Crystal data for 1: monoclinic, space group C2/c, a =18.945(4), b = 7.700(2), c = 11.888(2) (A), β = 101.67(3)°, V = 1698.3(6) (A)3, Z = 4, F(000) =760.0, Dc = 1.402 g/cm3, the final R = 0.0607 and wR = 0.1607 for 950 observed reflections (I ＞2σ(I)); and those for 2: monoclinic, space group P21/c, a = 17.982(1), b = 15.879 (1), c = 7.0716(5) (A), β = 100.675(1)°, V = 1984.3(3) (A)3, Z = 4, F(000) = 1010.0, Dc = 1.631 g/cm3, the final R = 0.0316 and wR = 0.0896 for 3784 observed reflections (I ＞2σ(I)). Crystal structure analysis indicates that in 1, molecules of L in a "V-shaped" conformation are linked to chains sustained by O-H…O hydrogen bonds between carboxylate groups and solvent water molecules.The chains are joined by O-H…O and C-H…O hydrogen bonds to further expand into a three-dimensional structure. For 2, molecules of L in a "Z-shaped" conformation are linked by hydrogen bonds between carboxylate groups and aqua ligands to form a chain of loops running down the b axis. The (2D→2D) polythreading in compound 2 represents the mode of parallel interpenetration of 2D sheets, having polyrotaxane character.     

Structural refinement of Nd[Fe(CN)6]·4H2O and study of NdFeO3 obtained by its oxidative thermal decomposition at very low temperatures

The crystal structure of Nd[Fe(CN)₆]·4H₂O has been refined by Rietveld analysis using high resolution synchrotron powder X-ray diffraction data. It belonged to the orthorhombic crystal system, Cmcm space group, with cell parameters: , and . The change in space group from P6₃/m which is observed in the pentahydrates (LnFe(CN)₆·5H₂O) to Cmcm in the tetrahydrates has been analyzed to be a consequence of the change in 9-fold coordination of Nd³⁺ in the pentahydrates to 8-fold coordination in the tetrahydrates, which changes the Nd³⁺ environment from tricapped trigonal prism to a distorted tricapped trigonal prism or square antiprism. Its decomposition process in air to produce NdFeO₃ has been followed by thermogravimetric and differential thermal analysis, IR spectroscopy and laboratory powder XRD. We found that it is possible to synthesize crystalline NdFeO₃ at temperatures as low as 380 °C and refine the structure of single phase crystalline NdFeO₃ synthesized by this method at 600 °C.     

[Cu3(μ10-bta)(μ2-C2O4)(H2O)2]n的水热合成与结构表征

有机-无机杂化材料因其在催化、化学吸附、磁性和电子导体等方面具有广泛的应用而成为人们的研究热点[1,2]. 通过过渡金属离子和特殊的有机配体之间的反应, 一系列具有独特结构的配位聚合物已被合成出来. 多齿有机配体可螯合两个或多个金属离子, 这些金属离子之间存在良好的电子交换[3], 可形成一维、二维或三维的配位聚合物. 均苯三甲酸和均苯四甲酸都是良好的桥连多齿配体, Chui等采用均苯三甲酸合成了具有吸附作用的大孔道的[Cu3(tma)2(H2O)]n[4] (tma=benzene-1,3,5-tricarb-oxylate)三维配位聚合物, 并且[Ni(C12H3ON6O2)]3(tma)*H2O[5], [M(tma)2]*12H2O(M=Co,Ni,Zn)[6], Na2[Co(H2O)6(bta)]*4H2O[7] (bta=benzene-1,2,4,5-tetracarboxylate)和[Co(phen)(md)][8] (phen=1,10-phenanthroline, md=benzene-1,3-dicarboxylate)等配位聚合物也先后被合成出来.     

Reactions of 3-cyclopropyl-3-oxopropionitrile anion generated by electroreduction of 5-cyclopropylisoxazole

3-Cyclopropyl-3-oxopropionitrile anion obtained by cathodic reduction of 5-cyclopropylisoxazole in an aprotic medium was used as an example to demonstrate that cyano ketone anions show a dual reactivity. The reaction of acetyl chloride with the electrogenerated tetrabutylammonium salt of 3-cyclopropyl-3-oxopropionitrile gave O-acylation products, whereas the reaction with its sodium salt gives C-acylation products. The reactions of these salts with hydroxylamine hydrochloride follow a different route: in the case of the tetrabutylammonium salt, resinification takes place, while in the case of the sodium salt, 5-amino-3-cyclopropylisoxazole is formed. The condensation of this product with 4,4,4-trifluoro-1-(2-thienyl)butane-1,3-dione in glacial AcOH affords 3-cyclopropyl-6-(2-thienyl)-4-(trifluoromethyl)isoxazolo[5,4-b]pyridine in 85% yield. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2110–2114, November, 2007.     

Direct Electrochemistry of Hemoglobin Immobilized in Sodium Alginate Film on the Ionic Liquid [BMIM]PF6 Modified Carbon Paste Electrode

In recent years the direct electron transfer of redox protein on electrode surface has attracted great attentions1. Different kind of modified electrode and various supporting films for immobilization of proteins had been proposed. But most of them are ba…     

非碱性介质中分子筛的合成

分子筛的合成通常是采用含碱金属离子的强碱性体系,通过水热晶化法实现~[1,2]的.得到的分子筛原粉不但必须通过铵离子交换和焙烧才能转变为氢型催化剂,而且在该体系中晶体的粒度也较小.Guth等人~[3]首次报道了在非碱性介质F-离子存在下直接合成铵型ZSM-5的工作.除用四丙基溴化铵合成ZSM-5及其杂原子分子筛外~[4],尚未见到在非碱性介质中合     

Synthesis and Crystal Structure of Ag2（admtrz）2（CF3CO2）2（admtrz=4—amino—3,5—dimethyl—1,2,4—triazole）

1 INTRODUCTION Transition metal complexes bridged by 1, 2, 4-triazole group can produce interesting structures and specific properties[1]. Many attempts have been made to synthesize a variety of complexes with paramagnetic centers by using such ligands, and their structures and magnetic properties have been characterized[2]. However, the polynuclear Ag(I) complexes bridged by 1, 2, 4-triazole have been poorly studied[3]. Recently, we have prepared a series of silver(I) triazole complex…