Hydration of complexes of 18-crown-6 with potassium nitrate or potassium picrate in the polymer phase

Adsorption of water vapor by granular polymer based on dibenzo-18-crown-6 and containing potassium nitrate or potassium picrate in the polymer phase was studied by the isopiestic method at 298 K. The adsorption of water vapor is described by isotherms corresponding (according to BDDT classification) to polymolecular absorption with a high adsorptive potential. In terms of the Aranovich model of polymolecular absorption, the monolayer capacity and differential heat of adsorption were calculated, and the stoichiometry of hydration of the potassium nitrate and potassium picrate complexes with immobilized crown ether was estimated. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 1940–1942, October, 1998.     

PHOTO-INDUCED DOPED POLYANILINE BY THE VINYLIDENE CHLORIDE AND METHYL ACRYLATE COPOLYMER AS PHOTO ACID GENERATOR

The emeraldine base form of polyaniline (PANI) can be doped by a photo-induceddoping method. In this method a copolymer of vinylidene chloride and methyl acrylate(VCMAC) was used as photo acid generator which can release proton when it is exposedto ultraviolet light (λ= 254 nm). The structure of PANI-VCMAC system before and afterirradiation was characterized by elemental analysis, IR, XPS, and SEM images. Resultsobtained indicate that the photo-induced doping characteristics, such as doping positionand type of charge carriers, are similar to that of PANI doped with HCl. The poor room-temperature conductivity (～10~(-5)S/cm) of PANI-VCMAC system after irradiation maybe due to low doping degree (～pH= 3) and the difference in morphology as compared withPANI-HCl film.     

Influence of conjugated nitrogenous bases on the spectra and structure of mixed-ligand nickel(II) chelates containing β-diones

The infrared and electronic excitation spectra of a series of new nickel(II) chelates containing an-diimine (or nitrogenous base, enR) and the anion of a-dione (1,3-ketoenol or 1,3-ketoester,H) were obtained in the solid state and in solution. The composition and the overall structure of the new chelates in the solid state depends on ligand concentration, the substituents within the-dionato moiety and the counterion present. The IR and electronic excitation spectra of [Ni(enR)₂ ]NO₃ and [Ni(enR)(O₂NO)] indicate, in conjunction with other physicochemical measurements, bidentate coordination of the ligands, while the spectral shifts reveal replacement of the (O,O)nitrato group by basic solvents. The existence of the nickel(II) in an octahedral environment is confirmed by an X-ray structure analysis of [Ni(dpamH)₂acac]NO₃ · CH₃OH (monoclinic, space groupP2_l/n, a=17.296(1),b=7.462(1),c=21.604(3) å,=95.65(1),Z=4, R=0.0534,Rw=0.0600), where dpamH denotes the 2,2-dipyridylamine.     

Crystal Structure of (6S,9S,13R,14S)-7,8-Didehydro-3,7-dimethoxy-17-methylmorphinan-4,6-diol

1 INTRODUCTION (9S,13R,14S)-7,8-Didehydro-3,7-dimethoxy-4-hydroxy-17-methylmorphinan-6-one I is an impor- tant natural product that was used to ease pain, decrease blood pressure and diminish inflammation. In order to study the stereochemistry of the reduction of I with potassium boronhydride, the crystal structure of the title compound II was determined by X-ray diffraction method. 2 EXPERIMENTAL 2. 1 Instrument The melting point was measured on a Yanagimoto MP-500 apparatus…     

酚酞型聚芳醚砜(Ⅶ):K_2C0_3存在下PP/DCDPS体系聚合反应机理的研究

利用~(13)C-NMR方法研究了弱碱K_2CO_3存在下酚酞成盐反应及其与活性双卤砜亲核缩聚反应过程中的结构特征。对一系列碱性条件下酚酞(PP)与4,4'-二氯二苯砜(DCDPS)的缩聚反应的研究表明任何影响内酯结构酚酞盐生成的因素都会严重阻碍聚合反应的进行。对模型化合物存在下K_2CO_3在极性非质子溶剂中的溶解/解离行为的研究结果表明酚酞类Card。双酚与固体K_2CO_3之间可能存在着一种特殊的络合作用。基于我们系列研究结果,本文中总结提出了弱碱K_2CO_3存在下酚酞的反应机理。     

Complexation of Ni (II) and Zn(II) ions by 3-(1-naphthyI)-2-mercaptopropenoic acid

The complexation equilibria between Ni(II) and Zn(II) metal ions with 3-(1-naphthyl)-2-mercaptopropenoic acid (H₂NMP) were studied by glass electrode potentiometry, at 25 °C and 1.0 mol·dm^–3 in NaClO₄ as constant ionic medium in 50% (v/v) water-ethanol solutions. Formation constants for the complexes Ni(NMP), Ni(NMP) ₂ ^2– , Zn(NMP) and Zn(NMP) ₂ ^2– , refined by the MINIGLASS program, are reported.     

Gem-dinitro compounds in organic synthesis. 4. Use of the condensation product of glyoxal and dinitromethane in the synthesis of nitro-1,2,3-triazoles

The condensation of dinitromethane with glyoxal has been investigated and it has been demonstrated that 1,1,4,4-tetranitro-2,3-butandiol, -hydroxy-,-dinitropropionic acid or their mixture may be formed. Interaction of 1,1,4,4-tetranitro-2,3-butandiol or 1,4-dibromo-1,1,4,4-tetranitro-2,3-butanediol diacetates with sodium azide leads to bis(5-nitro-1,2,3-triazol-4-yl) via intermediate 1,1,4,4-tetranitro-1,3-butadiene.For communication 3, see [1].N. D. Zelinskii Institute of Organic Chemistry, Russian Academy of Sciences, 117913 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 9, pp. 2123–2131, September, 1992.     

Strukturelle Abwandlungen anN-Acetylneuraminsäure, 3

From methyl-5-acetylamino-7,8-anhydro-4,9-O-bis-(t-butyldimethylsilyl)-3,5-dideoxy--D-glycero-D-galacto-2-nonulopyranosidonic acid methylester (1) the derivatives1 a and1 b were obtained by removing the 9-O-(t-butyldimethylsilyl)group withBu ₄NF, followed by acetylation. Treatment of1 b with 80% acetic acid and acetanhydride/pyridine yields the 8-epi-N-acetylneuraminic acid derivative2 a and the 7-epi-N-acetylneuraminic acid derivative3 a in a ratio of 3:1 (Scheme 1). The structure elucidation of2 b was achieved by converting2 b via the 4,9-bis-O-(tBDMSi)-8-O-tosyl-derivative2 d into the epoxide1 (Scheme 2). Using the same sequence the epoxides4 and5 were transformed into theN-acetylneuraminic acid derivative6 a and the 7,8-bis-epi-N-acetylneuraminic acid derivative7 a (Scheme 3). After treatment with sodium hydroxide and 0.025m HCl and Dowex 50 H⁺ the 8-epi-, 7-epi- and 7,8-bis-epi-N-acetylneuraminic acids2,3, and7 were obtained. These three compounds were tested withCMP-N-acetylneuraminic acid synthetase.

Herrn KollegenK. Schlögl mit den besten Wünschen zum 60. Geburtstag.     

密闭微波辅助萃取当归粉中的阿魏酸

利用密闭微波样品制备系统(具有压力控制部件),对当归中的有效成分阿魏酸的萃取进行研究,比较了密闭微波萃取同超声波萃取和索氏萃取阿魏酸提取率的差异.结果表明:微波萃取与其他两种萃取方法相比,具有速度快和萃取率高的特点.并得到了阿魏酸提取的最佳条件:微波功率为400 W,萃取剂为90%的乙醇(体积分数),固-液比为1∶15,微波辐射为240 s,当归粒径为75μm.     

BaCe0.8Ho0.2O3-a陶瓷的性质与应用

Ceramic BaCe0.8Ho0.2O3-α with orthorhombic perovskite structure was prepared by conventional solid state reaction, and its conductivity and ionic transport number were measured by ac impedance spectroscopy and gas concentration cell methods in the temperature range of 600-1000 ℃ in wet hydrogen and wet air, respectively. Using the ceramics as solid electrolyte and porous platinum as electrodes, the hydrogen-air fuel cell was constructed, and the cell performance at temperature from 600-1000 ℃ was examined. The results indicate that the specimen was a pure protonic conductor with the protonic transport number of 1 at temperature from 600-900 ℃ in wet hydrogen, a mixed conductor of proton and electron with the protonic transport number of 0.99 at 1000 ℃. The electronic conduction could be neglected in this case, thus the total conductivity in wet hydrogen was approximately regarded as protonic conductivity. In wet air, the specimen was a mixed conductor of proton, oxide ion and electron hole. The protonic transport numbers were 0.01-0.09, and the oxide-ionic transport numbers were 0.27-0.32. The oxide ionic conductivity was increased with the increase of temperature, but the protonic conductivity displayed a maximum at 900 ℃, due to the combined increase in mobility and depletion of the carriers. The fuel cell could work stably. At 1000 ℃, the maximum short-circuit current density and power output density were 346 mA/cm^2 and 80 mW/cm^2, respectively.