中国化学快报

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A New Metallomicelle with Hydrolytic Metalloenzymatic Activity

Qiu Yun, DAI Yun, Du Deng

中国化学快报. 1996, 7(10): 879-880.

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可视化

A new metallomicelle, formed by Cu²⁺ or Zn^2- ion and N-tetradecyl-2-(N-2-hydroxyethyl aminomethyl) imidazol in the presence of ceryltrimethylammonium bromide, was found to possess remarkable catalytic activity to the hydrolysis of p-nitrophenyl picolinate.

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Synthesis of New 1, 6-disubstituted Fulvenes

Hu XIAO, Shu Feng, CHEN, Xiao, Tian LIANG

中国化学快报. 1996, 7(10): 881-883.

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Sixteen new 1, 6-disubstituted fulvenes have been prepared by acylation of cyclopentadienyl sodium and the result of preliminary pharmacological tests showed that several of them have antineoplastic activity.

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The Synthesis and Structure of Adduct of a New Schiff Base Macrocycle with Two THF:THIONE₂B₄［36］ENE-O₆N₈·2THF

Zhen Guang LIN, Hua Yang CHEN, Yu Juan LIN, Feng Hua HUANG

中国化学快报. 1996, 7(10): 884-885.

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New Schiff base Macrocyclic compound of 2, 3:11, 12:20, 21:29, 30-tetrabenzo-l, 13, 16, 19, 31, 34-hexaoxa-5, 6, 8, 9, 23, 24, 26, 27-octaaza-7, 25-dithione-2, 3:4, 5:9, 10:11, 12:22, 23:27, 28:29, 30-cyclo-[36]ene (thione₂B₄[36]ene-O₆N₈) containing THF has been prepared.It crystallizes in the monoclinic, space group P21/n, with parameters a=9.829(5)Å, b=24.23(1)Å, c=10.181(9)Å, β =92.93(5)°, Z=2, V=2422(3)Å³, D_c=1.25gcm^-3.Data collection:Rigaku AFC-5R diffractometer, (MoK_α, λ =0.71069?), ω/2θ scans, θ_max=25°, empirical absorption correction, 4658 measured reflections, 4387 independent, 1743 observed reflections [I≥ 3σ(I)].The final R=0.056, R_W=0.069, S=1.54, (△/σ)_max=0.01, △ρ_max=0.36eÅ^-3.

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Semisynthesis and Biological Evaluation of Taxayuntin 13-［N-Benzoyl-(2'R,3'S)-3'-phenylisoserinate］

Qin YUE, Qi Cheng FANG, Xiao Tian LIANG

中国化学快报. 1996, 7(10): 886-887.

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A novel taxol analog with 5/7/6/4 skeleton, taxayuntin 13-[N-benzoyl-(2'R, 3'S)-3'-phenylisoserinate](8) was semisynthesized with an ED₅₀ of 11.0 μg/ml in cytotoxicity assay against KB cell line.

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The Synthesis of Hexamethyl Ether of Salvianolic Acid A Benzyl Ester

Yan ZHUANG, Zong Ru GUO, Guang Zhong YANG, Xiao Tian LIANG

中国化学快报. 1996, 7(10): 888-891.

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A salvianolic acid A derivative, hexamethyl ether of salvianolic acid A benzyl ester, was synthesized in fourteen steps.The overall yield was 3.4‰.The compound was identified by ¹HNMR and MS.This is the first report of building this structural skeleton.

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Study on the Total Synthesis of Hainanolide-Construction of Tricyclic Intermediate(I)

Lu Yan ZHANG, Shi Zhi CHEN, Dong WEI, Liang HUANG, Ji Jie CHAI, Cun Heng HE

中国化学快报. 1996, 7(10): 892-893.

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Tricyclic compounds (4b-endo) and (4b-exo) are synthesized as the plausible intermediates of the total synhthesis of hainanolide by Lewis acid catalyzed intramolecular Diels-Alder (IMDA) reaction.

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Synthesis of 1, 3-cyclic Monoalkyl(acyl)-racglycerothiophosphates of Uridine

Cheng Xiang ZHANG, Ru Yu CHEN, Chu Chi TANG, Huan Ming CHEN

中国化学快报. 1996, 7(10): 894-895.

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New structural phospholipids 1, 3-cyclic monoalkyl(acyl)-rac-glycerothiophosphates of uridine were synthesized.The strategy for the synthesis is using hexaethylphosphorous triamide, activated by a catalytic amount of iodine, as the phosphorylating reagent.Their structures were confirmed by ¹HNMR, ³¹PNMR, IR and elemental analysis.

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Total Synthesis of dl-Ligustiphenol

Yan He HUANG, De Quan YU

中国化学快报. 1996, 7(10): 896-897.

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—(-)S-Ligustiphenol is a new sesquiterpene compound with antiinflammatory and immunosuppressive activities.The total synthesis of its racemate was carried out by a six-step reaction sequence including bromination of aldehyde, iodination of m-cresol, protection of phenolic hydroxyl, Grignard reaction, aldol condensation, etc.The target compound was characterized by comparing its ¹H NMR, MS and IR spectra with natural (-) ligustiphenol.

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Unusual Aromatization of 9-methyl-6-oxo-5-tosyl-6a, 7, 8, 10a-tetrahydroinden[2,3-b]indole

Qian CHENG, Xiao Tian LIANG, Jingle Xi XIE

中国化学快报. 1996, 7(10): 898-899.

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9-Methyl-6-oxo-5-tosyl-6a,7,8,10a-tetrahydroindeno[2,3,b]indole (Ⅱ) was aromatized by PPE, CF₃COOH or BF₃·Et₂O to furnish the new compound, 9-methyl-5-tosyl-6H-indeno[2,3,b]indole (Ⅷ), involving an unusual"dehydration";the loss of two H's and concomitant exocyclic (to the aromatized carbocycle) removal of the carbonylic oxygen.

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The Synthesis of 1-(4-(N-methylsulfamylmethyl)phenyl-4-ethoxycarbonyl-2-methyl-pyrrole．A New Method of Pyrrole Synthesis

Yan ZHANG, Yun Zhen JIANG, Xiao Tian LIANG

中国化学快报. 1996, 7(10): 900-901.

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Under basic conditions 4-(N-methyl-sullamylmethyl)aniline 1 reacted with ethyl 3-bromopyruvate 2 in acetone to give the title compound 5.The structure of 5 was established by MS, IR, ¹HNMR and ¹³CNMR spectra.

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Base-Catalyzed Rearrangement of 11-Isopropylidene-anti-4,5-Epoxy-endo-Tricyclo［6. 2. 1. 0^2,7］ Undeca-4,9-Diene-3,6-Dione

Xiao Pei GUAN, Jian Guang SUN, Yong Zhong YU

中国化学快报. 1996, 7(10): 902-904.

摘要 ( )

可视化

Treatment of 11-isopropylidene-anti-4, 5-epoxy-endo-tricyclo[6.2.1.0^2,7] undeca-4, 9-diene-3, 6-dione(6) with methanolic sodium hydroxide results in Favorskii-type ring contraction with concomitant Cope rearrangement and Haller-Bauer cleavage, thereby affording dimethyl-9-isopropxlidene-cis-bicyclo[4.3.0] nonane-(2S)-2, 3-dicarboxylate (7) as the ultimate product.The structure of 7 was confirmed by single crystal X-ray analysis.

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Formation of Dithymidylic Acid by Ester Exchange Reaction on N-Phosphoryl Serine

Yuan MA, Xiang Hong LI, Yi CHEN, Yu Ping FENG, Yu Fen ZHAO

中国化学快报. 1996, 7(10): 905-906.

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Ester exchange reaction between the thymidine and N-(O, O-diisopropyl)phosphoryl serine could yield several derivatives of thymidylic acid, including dithymidylic acid.These results might be meaningful to the prebiotic synthesis of macromolecules.

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A New Convenient Synthesis of Pyridine-N-oxides

Tao LU, Xin Zhong SHI, Yi Ming WU

中国化学快报. 1996, 7(10): 907-908.

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This paper describes the direct oxidation of pyridines to pyridine-N-oxides by means of 30% H₂O₂ in aq media in the presence of Na₂WO₄.2H₂O as catalyst instead of with per-acids or 30% H₂O₂ in acetic acid.Good yields were obtained.

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More Feasible Way to Cleave Photo-Labile Resin

De Xin WANG, Yu Hong GUO, Lei HUANG

中国化学快报. 1996, 7(10): 909-910.

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A combinatorial cleavage, acidolysis-saponification, after solid phase peptide synthesis on photo-labile resin was stated in present paper.Peptide (Gly-Asp-Ala-Lys-Gly)₂ > Lys-OH was liberated with high yield(92.1%) and excellent purity(91.6%) from its protected peptidyl nitro-resin precursor by a new orthorgonal protocol:1) Hi-TFMSA, 2) 0.2N NaOH/90% EtOH.

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Two New Sesquiterpenes from Ligularia Dentata

Kun GAO, Li YANG, Zhong-Jian JIA

中国化学快报. 1996, 7(10): 911-912.

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Two new germacrane sesquiterpenes(1) and (2) were isolated from Ligularia dentata.Their structures were elucidated by spectroscopic methods and 2D-NMR techniques.

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New Sesquiterpene from Senecio flammeus

Jin Feng HU, Su Ping BAI, Zhong Jian JIA

中国化学快报. 1996, 7(10): 913-914.

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A new eudesmane sesquiterpene 1β, 4β, 6α, 15-tetrahydroxyeudesmane isolated from Senecio flammeus and its structure determined on the basis of spectral data are reported.

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New Benzodioxin from Ligularia Intermedia Nakai

Bin MA, Yan Ping SHI, Zhong Jian JIA

中国化学快报. 1996, 7(10): 915-916.

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A benzodioxin derivative was isolated in the phytochemical investigation of Ligularia intermedia Nakai.Its structure was elucidated by high field ¹H NMR, ¹³C NMR and DEPT, together with the EI-MS and IR.

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12-Deoxyphorbol Esters from Euphorbia Fischeriana

Wen Zi LIU, Xiao Yun WU, Gen Jin YANG, Qing Gao MA, Tian Xi ZHOU, Xi Can TANG, Guo Wei QIN

中国化学快报. 1996, 7(10): 917-918.

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Two compounds, 12-deoxyphorbol-13-hexadecanoate 1 and 12-deoxyphorbol-13-acetate 2 were isolated from the roots of Euphorbia fischeriana.Compoound 1 was elucidated as a new diterpenoid.Compound 2 was discovered for the first time from this plant and showed analgesic and sedative activities in preliminary experiment in mice.

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Application of H-point Standard Additions Method in Fluorescence Analysis-Simultaneous Determination of α-Naphthol and β-Naphthol

Jing Tian HU, Jing He YANO, Wen Yuan MA, Guang Jun ZHOU, Rong Jiang HAN

中国化学快报. 1996, 7(10): 919-921.

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The H-point standard additions method is applied in fluorimetry for determining α-naphthol and β-naphthol simultaneously.When the concentration ratio of α-naphthol to β-naphthol in the sample varies from 40:1 to 1:20, the accuracy and precision of the results are both satisfactory.

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New Polarographic Immunoassay Using Copper Ion as Catalyst for Conversion of Substrate Instead of Natural Enzyme

Jun Feng SONG, Jian Xiu WANG, Wei GUO, Min Ren ZHAO

中国化学快报. 1996, 7(10): 922-923.

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A new electrochemical immunoassay based on catalytic conversion of substrate by labeled metal ion and polarographic detection of generated product was developed.In this immunoassay, copper ion was used A catalyst for the conversion of substrate to substitute natural enzyme.Copper ion was labeled to antigens such as Human serum albumin( HSA ), Diphtheria Toxoid ( DT ), Tetanus Toxoid ( TT ) through bifunctional chelating agent diethylenetriamine pentaacetic acid ( DTPA ).After heterogeneous competitive immune reaction, the labeled copper ion was released by acidification, and then catalyzes chemically the conversion of substrate o-phenyldiamine ( OPD ) to electroactive product 2, 3-diaminophenazine ( DAP ).The product DAP was detected by using linearsweep polarography.The sensitivity of the proposed assay for the determination of HSA, DT and TT is superior to those of previous one based on direct detection of the labeled metal ion.

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Study on the Singlet and Triplet StateElectron Transfer between Hypocrellin A and Aromatic Amines in Solvents of Various Polarity

Min WENG, ManHua ZHANG, Tao SHEN

中国化学快报. 1996, 7(10): 924-927.

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In this paper, the singlet and triplet state electron transfer processes between hypocrellin A(HA) and aromatic amines in solvents of various polarity have been studied by fluorescence and time-resolved transient absorption spectra.The results show, in.polar solvent, the quenching of HA fluorescence by aromatic amines results in Stern-Volmer plot, the investigation of transient absorption indicated that triplet-state electron transfer process from ³HA^* to the ground-state of amines occured, and the values of the singlet and triplet state electron transfer rate constant were calculated, however in weak polar solvent, only the triplet-triplet absorption of HA was observed.

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Oscillation in the KMnO₄-NH₂CH₂COOH CSTR System

He Xing LI, Xiao Jun HUANG

中国化学快报. 1996, 7(10): 928-930.

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The chemical oscillating reactions in KMnO₄-NH₂CH₂COOH-H₃-PO₄ CSTR system in the presence and absence of Ag⁺ have been studied.The reaction conditions and phase diagrams have been determined.Some effects on the oscillation have been studied.The stabilization of colloidal particles of MnO₂ by PO₄^3- has been investigated.The roles of Ag⁺ in the above reactions have also been studied.

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Photoinduced Intramolecular Electron Transfer in an Oblique Zinc Phthalocyanine-Viologen Linked System

Hong Jian TIAN, Qing Fu ZHOU, Hui Jun XU

中国化学快报. 1996, 7(10): 931-934.

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The spectroscopic properties and photoinduced electron transfer process have been studied in zinc phthalocyanine-viologen system with bisphenol A (ZnPcAV²⁺).It was found that the excited singlet state of zinc phthalocyanine moiety is quenched and the fluorescence lifetime is reduced by the linked viologen.Nanosecond laser photolysis studies showed that intramolecular quenching of the excited triplet state of zinc phthalocyanine moiety by the attached viologen occurred giving reduced viologen radical ion (V⁺) that survived over 50μs.

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The Enhancement of Fluorescence of The Squaraine Dye LB Films by Overcoating of Glycolipids

Jin Ru LI, Chang Yu FAN, Bao Fang LI, Long JIANG

中国化学快报. 1996, 7(10): 935-938.

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The influence of overcoating layers of dialkylglycerylether-β-glucosides(A), 1,2-O-dialkylglycerylethers(B) and.arachidic acid (C₂₀) on the fluorescence of the squaraine dye(SQ) and C₂₀ mixed film were investigated by fluorescence and time-resolved fluorescence measurements.An apparent increase in fluorescence intensity for three layer mixed film of SQ and C₂₀ were obtained by overcoating A in comparison with the small change fluorescence intensity for SQ dye mixed film by overcoating B or C₂₀.

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Cooper and Zinc Superoxide dismutase from Peking duck erythrocytes forms a supramolecular double-helix in the crystal

Ping Wei LI, Yu LUO, Gen Pei LI, Mei Cheng SHAO

中国化学快报. 1996, 7(10): 939-941.

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The charge isomer fraction(PI 5.9) of the Cu.Zn SOD from duck red blood cell has been crystallized around neutral pH and low ionic strength at 297K.The crystals belong to the trigonel space group P3₂21, with unit cell a=125.lÅ, c=163.3A and γ=120°.The duck SOD shows a novel packing arrangement consisting of supramolecular double-helix, with 9₂2/9₇2 non-crystallographic border group symmetry in the crystal.

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Structure of Atactic Polystyrene Film Formed from aPS/CS₂ Gel

Yan Xiang WANG, Wen Hui SONG, De Yan SHEN

中国化学快报. 1996, 7(10): 942-943.

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Novel ordered structure was detected in atactic polystyrene(aPS) formed from aPS/CS₂ gel, the ordered structure is constructed through stacks of stereoregular segments by accepting TTGG type conformation.Another anomalous phenomenon was that many particles with different shape and size formed on surface of the film, these were some special aggregates with more ordered structure.

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Photophysical Behaviors of Azobenzene in Solvent-Swollen Nafion Membranes

Jing Qu GUAN, Chen Ho TUNG

中国化学快报. 1996, 7(10): 944-947.

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The fluorescence from azobenzene (AB) molecule incorporated into water-swollen Nafion in acid form was observed at room temperature for the first time.The incorporation process was investigated by UV absorption.The plot of the concentration of AB in Nafion vs.the soaking time shows that the adsorption process is diffusion-controlled, and the apparent diffusion coefficient (D) was determined to be 7.6×10¹⁰cm²s^-1.These results are attributed to the fact that AB molecules are located in the fluorocarbon/water interface of the Nafion membranes and are protonated.In methanol-swollen Nafion membranes, AB fails to fluoresce because it is located at the methanol pool enclosed by the cluster networks.

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Morphology of Branch Chain in Copolymer Surfactants on Interface

Jian XU, Liang He SHI, Mei Ling YE

中国化学快报. 1996, 7(10): 948-950.

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The conformation of amphiphilic branch chain in acrylamide-poly(oxyethylene alkyl ether)acrylate copolymers on interface was investigated by static laser light scattering and X-ray photoelectron spectroscopy.The results show that the conformation of branch chain alters with copolymer structure.

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Interaction of Polyelectrolyte with Fluorocarbon Surfactant in Aqueous Solution

Yong Zhi WANG, Hai Feng JI, Chen Ho TUNG, Gui Chun YUE

中国化学快报. 1996, 7(10): 951-953.

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The variation of the I₁/I₃ ratio of the fluorescence of pyrene in polystyrene-based quaternary ammonium salt (PA) and sodium carboxymethylamylose (NaCMA) aqueous solutions was measured as a function of sodium perfluorooctanoate (SPFO) concentration.Association of the anionic fluorocarbon surfactant with cationic polyelectrolyte (PA) to form mixed micelles occurred at the surfactant concentrations far below its normal critical concentration, while no interaction between SPFO and anionic polyelectrolyte (NaCMA) was detected.The driving force for the formation of mixed micelles of SPFO and PA is electrostatic interactions.

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Study of Binary Rare-Earth Oxyfluoride for ODE Reaction and Their XRD &In-Situ Raman Characterization

Ji Zhong LUO, Xiao Ping ZHOU, Zi Sheng CHAO, Hu Lin WAN

中国化学快报. 1996, 7(10): 954-955.

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A series of new binary rare earth oxyfluoride ( Sm₂O₃-LaF₃ ) catalysts have been developed for ODE reaction.High C₂H₄ selectivity (91.5%) with C₂H₆ conversion 21.7% was achieved on the catalyst Sm₂O₃/LaF₃ with molar ratio 1/1 at 700℃.The addition of 16.7 mol % BaF₂ into Sm₂O₃/LaF₃(1/1 in mol) led to the increase of C₂H₆ conversion from 21.7% to 40.8%, however, the change of ethene seletivity was not apparent (from 91.5% to 88.0%).

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Novel Type CO₂ Methanation Catalysts over Ni/Sepiolite and Ru/Sepiolite System

Guo Cai DENG, Li XU, Rui Cai MU, Rong Ti CHEN, Wei LU

中国化学快报. 1996, 7(10): 956-959.

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可视化

A Novel type single-component catalyst in which small amounts of nickel of ruthenium supported on sepiolite was found to be a very efficient methanation catalyst for carbon dioxide at high space velocity.

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Structure of Activity Sites in Perovskite-type Complexs Oxides LaMnO_3＋λ for Total Oxidation of Methane

Zi Yi ZHONG, Jian GONG, Qi Jie YAN, Xian Cai Fu

中国化学快报. 1996, 7(10): 960-961.

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可视化

Nanometer oxide LaMnO_3+λ and its counterparts with large particle size were comparatively studied for total oxidation of methane.XPS, TPR and nonstoichiometric oxygen(λ) analysis results identify that the nanometer oxide contains more high valence cations, to which the adjacent lattice oxygen are responsible for total oxidation of methane at low temperature.

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A Methane Monooxygenase-like DinuclearIron (Ⅲ) Complex and its Catalytic Ability for Asymmetric Epoxidation of Styrene

Jun Fa WEI, Xian Da YU, Dao Sen JIN

中国化学快报. 1996, 7(10): 962-964.

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可视化

A methane monooxygenase-like dinuclear complex of iron (Ⅲ) with a chiral heptadentate ligand has been synthesed and tested for catalytic ability for asymmetric epoxidation of styrene with iodosylbenzene.The results show that the complex exhibits many qualitative features, such as electronic spectrum, catalytic behavior, and asymmetric induction similar to those of methane monooxygenase and catalyzes styrene epoxidation to R-(+)-styrene oxide in 9.3% yield and 72.9% optical yield.

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In Situ Confocal Microprobe Raman Spectroscopy Study of the Oxygen Species over Cerium Oxide

Rui Qiang LONG, Hui Lin WAN

中国化学快报. 1996, 7(10): 965-966.

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可视化

In situ confocal microprobe Raman spectroscopy results showed that O₂^2-, O₂^- and O₂^δ- (0 <δ< 1) adspecies formed on the O₂ pretreated cerium oxide sample when the temperature was below 423 K.At 1023 K, only CeO₂ F_2g peak (at 449 cm^-1) and O₂^- species (at 1159 cm^-1) were observed on the surface.The reactivity of methane with the oxygen species was lower than that of ethane with the oxygen species.

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Infrared Isotopic Shift of Lithium Carbonate and Sulfate

Wen TIAN, Jin Guang WU, Tsing Lien CHANG

中国化学快报. 1996, 7(10): 967-968.

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可视化

The Infrared spectea of ⁶Li₂CO₃, ⁷Li₂CO₃, ⁶Li₂SO₄, and ⁷Li₂SO₄ were studied.The isotopic shift of the vibrational frequency for ⁶Li-O and ⁷Li-O bonds amounts to 4.5-7.8 % for the carbonate and 9.5-11.6% for the sulfate.

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The Atomic Weight of Gadolinium, Dysprosium and Erbium

Tsing Lien CHANG, Ding Shun GAO

中国化学快报. 1996, 7(10): 969-972.

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可视化

Isotopic ratio measurement was made for gadolinium, utilizing the bias correction facor of cerium and europium for the same mass spectrometer.The atomic weight found from the raw data is A_r(Gd)=157.2473(2).However, the application of the method of double substitute calibration results in A_r(Gd)=157.2526(10), both on 2σ basis.For dysprosium and erbium, the same method yields A_r(Dy)=162.4993(10) and A_r(Er)=167.2611(12).

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1996年, 第7卷, 第10期　刊出日期：1996-10-20

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1996年, 第7卷, 第10期 刊出日期：1996-10-20

1996年, 第7卷, 第10期　刊出日期：1996-10-20