中国化学快报

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A CONVENIENT PROCEDURE TO PREPARE TRICYCLODECANE

Xiao Tun YANG, Jie ZHENG, Mei Yu HUANG, Ying Yan JIANG

中国化学快报. 1995, 6(01): 1-4.

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A magnesium oxide suppported-polytitazane-platinum complex has been prepared and used to catalyze the hydrogenation of dicyclopentadiene.This complex was very active and stable in the reaction.Dicyclopentadiene could be completely hydrogenated to tricyclo[5.2.1.0^2,6]decane in 100% yield at 60℃ and under atmospheric hydrogen pressure.

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REACTION OF HETEROCYCLIC KETENE AMINALS WITH DICHLOROCARBENE

Zhi Tang HUANG, Jian Chao, WANG, Li Ben WANG

中国化学快报. 1995, 6(01): 5-8.

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Heterocyclic ketene aminals 1 or 2 react with dichlorocarbene to give the formyl substituted heterocyhc ketene aminals 3 or 4 through the carbene insertion reaction of the α-C-H.

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EFFECTS OF RATE OF ADDITION AND TENIPERATURE ON THE ENANTIOSELECTIVITY IN BORANE REDUCTION OF KETONES CATALYZED BY CHIRAL OXAZABOROLIDINE

Yao Zhong JIANG, Yong QIN, Ai Qiao MI

中国化学快报. 1995, 6(01): 9-12.

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The excellent enantioselectivity with o.p.>99% in asymmetric borane reduction of acetophenone catalyzed by (4S,5R) 4,5-diphenyl-1,3,2-oxazaborolidine has been achieved via the important modification of the reaction conditions.

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A NOVEL SYNTHESIS OF 3-PHENYL-1H-INDAZOLE DERIVATIVES

Zhen Qi ZHONG, Yu Zhu QUI, Zheng ZHANG, Hong Wen Hu

中国化学快报. 1995, 6(01): 13-16.

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A facile,novel and one-pot method for the preparation of 3-phenyl-1H-lndazole derivatives in moderate yields by cyclization of the ortho-substituted benzophenone hydrazones in the presence of polyphosphoric acid (PPA) is reported.

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A NOVEL SILACARBOCYANINE DYE

Yao Jun ZHANG, Ji Xiang HAO, Zu Xun ZHANG

中国化学快报. 1995, 6(01): 17-18.

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A new type of photographic spectral sensitizer containing silicon-carbon double bond is reported.The application tests show that the dye has excellent sensitivity in silver iodobromide emulsion and that the sensitivity maximum (S_max) of emulsion sensitized by the dye gives a hypsochromic shift about 70nm as compared with the absorption maximum (λ_max) of the dye in methanol.This phenomenon differs entirely from typical photographic spectral sensitizing dye.

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STUDIES ON THE SYNTHESIS AND REACTIONS OF N－(1－OXO－4－CARBONYL－2,6,7－TRIOXA－1－PHOSPHABICYCLO ［2．2．2］ OCTANE)－N'－ARYL THIOUREAS

Yu Gui LI, Xue Feng ZHU

中国化学快报. 1995, 6(01): 19-22.

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N-(1-oxo-4-carbonyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2] octane)-N'-aryl thioureas(4) were synthesized in this paper.(4) reacted with AgNO₃-H₂O and chloroacetyl chloride to afford the corresponding urea derivatives (5) and cyclired products (10),respectively.The mechanism of desulphurisation of (4) has also been studied.

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THE SYNTHESIS OF O－MONOSACCHARIDYL－METHOXYCARBONYLPHOSPHONAMIDATES BY ARBUZOV REACTION

Ru Yu CHEN, Xiao Ru CHEN, Hut LI

中国化学快报. 1995, 6(01): 23-26.

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For the synthesis of O-monosaccharidyl-methoxycarbonylphosphonamidates,a new method in which Arbuzov reaction of monosaccharidylphosphoramidite with methyl chloroformate is the key step,is reported.Thus,a number of novel O-monosaccharidyl-methoxycarbonyiphosphonamidates were obtained successfully.

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PHOTOCHEMISTRY OF SUBSTITUTED PHENYL PHENYLACETATES WITHIN CYCLODEXTRIN CAVITIES

chen Ho TUNG, Yun Ming YING, Zhi Qiang YANG, Xiao Hong WANG

中国化学快报. 1995, 6(01): 27-30.

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The photochemical reactions of several substituted phenyl phenylacetates incorporated in the cavities of α-and β-cyclodextrins and in organic solvents were investigated.Photolysis of these esters in organic solutions results in both photo-Fries rearrangement and photodecarbonylation products.However,the esters included in cyclodextrin cavities almost exclusively undergo photo-Fries reactions.Furthermore,in the photo-Fries reactions of the inclusion complex the ratios of ortho to para rearrangement products are evidently increased compared with those in organic solutions.Those are good examples for using cyclodextrins to control the selectivity in photochemical reactions.

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EVIDENCE FOR AGGREGATE FORMATION OF LONG CHAIN PERFLUOROCARBON IN AQUEOUS ORGANIC SOLVENTS:EXCIMER EMISSION AND ENERGY TRANSFER

Chen Ho TUNG, HaI Feng JI

中国化学快报. 1995, 6(01): 31-34.

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In aqueous organic solvents perfluoroalkyl 2-naphthoates (NpFCn) with long fluorocarbon chain show strong excimer fluorescence.Excitation of NpFCn in the mixed solution of NpFCn and 9-anthrylmethyl perf1uoroalkanoates (AnFCn) results in strong emission of AnFCn.These observations suggest that hydrophobic interactions force fluorocarbon molecules to form aggregates.

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SYNTHESES OF Ph AND TEMPERATURE－SENSITIVE HYDROGELS AND THEIR APPLICATIONS IN CONTROLLED RELEASE OF BIOMACROMOLECULES

Feng LIU, Feng Hua LIU, Guo Liang TAO, Rem Xi ZHUO

中国化学快报. 1995, 6(01): 35-38.

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A series of pH-and temperature-sensitive hydrogels were prepared.These gels do not swell at 37℃ and pH 1.4 but swell at 37℃ and pH 7.4.When papain was loaded in these gels,it can be released at 37℃ and pH 7.4 in a high percentage without any loss of activity.

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CYCLOPEPTIDE FROM THE SEEDS OF ANNONA GLABRA

Chao Ming LI, Ning Hua TAN, Hui Lan ZHENG, Xiao Jiang HAO, Jun ZHOU

中国化学快报. 1995, 6(01): 39-40.

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A new cyclopeptide glabrin A has been isolated from the seeds of Annona glabra.Its structure was elucidated by 2D-NMR and FAB-MS.

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STRUCTURE ELUCIDATION AND SYNTHESIS OF CONISELIN FROM CONISELIUM VAGINATUM THELL

Ping Yu DING, Ruo Yun CHEN, De Duan YU

中国化学快报. 1995, 6(01): 41-44.

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Coniselin,a new natural compound,was isolated from the roots of Coniselium Vaqinatum Thell.Its structure was elucidated by means of spectroscopic analysis (UV,IR,MS,NMR,DEPT) and confirmed by total synthesis.

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MURICATALIN, A NEW POLYKETIDE FROM ANNONA MURICATA (ANNONACEAE)

Hua Qing GUI, jing Guang YU, Zhi Li YU

中国化学快报. 1995, 6(01): 45-48.

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Muricatalin (1),a new polyketide (acetogenin) has been isolated from Annona muricata L.Its structure and relative stereochemistry were elucidated on the basis of the spectral analyses of 1 and its derivatives,the acetate (2) and the mesitoate (3)

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DYNAMIC OSCILLOGRAPHIC ANALYSIS

Peng LIU, Jian Bin ZHENG, Sheng Hua SHI

中国化学快报. 1995, 6(01): 49-52.

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Dynamic oscillographic analysis means the combination of flow injection technique with oscillographic analysis,and oscillographic determination is carried out in continuously flowing solution.Oscillograms obtained in this way have good stability and high reproducibility.Thus,oscillographic determination method will become really feasible analyti-cal method.

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TWO NOVEL EASILY PREPARED CHIRAL POLYSILOXANE STATIONARY PHASES FOR GC RESOLUTION OF ENANTIOMERS

Xi Chun ZHOU, Xue Ran LU, cai Ying WU, Yuan Yin Chen

中国化学快报. 1995, 6(01): 53-54.

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Two new substituted chiral polysiloxanes were synthesized by the reaction of polymethylhydrosiloxane with chiral moieties containing alkenes derived from D-tartaric acid and L-phenylalanine.The primary GC characteristics of the two phases were also determined.

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THE STUDY ON IN VITRO METABOLISM OF BUTYLPHTHALIDE BY GAS CHROMATOGRAPHY－MASS SPECTROMETRY

Shi Hua PENG, Tong Hui ZHOU

中国化学快报. 1995, 6(01): 55-58.

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The in vitro metabolism o.butylphthalide (HBP) by rat liver microsomes was studied in this paper.Capillary GC/MS and BSTFA/1%TMCS derivatization were used for the separation and structure identification of the six metabolites.3-Hydroxylation and r-hydroxylation have been proved to be the main metabolism pathways of HBP by rat liver microsomes.

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THE CALCULATION OF RATE CONSTANT OF ELECTRON TRANSFER REACTION AT ELECTRODES

Yin Sheng WU, Zheng Yu ZHOU, Ai Ping FU

中国化学快报. 1995, 6(01): 59-62.

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After the electron transfers from the metal electrode to the Fe³⁺(H₂O)₆ ion,the free energy of activation of this electron transfer reaction is calculated,then using the transition probability which is calculated by the perturbed degeneration theory and the Fermi golden rule,the rate constant is gotten.Compared with the experimental results,it is satisfactory.

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INVESTIGATION ON THE WATER－SOLUBLE YTTERBIUM PORPHYRIN PARTⅡ THE ELECTROCHEMICAL STUDY OF THE YTTERBIUM PORPHYRIN COMPLEX

Qian Kun ZHUANG, Xiao Xia GAO

中国化学快报. 1995, 6(01): 63-66.

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A two-electron irreversible adsorptive reduction peak was observed for the water-soluble ytterbium complex by cyclic voltammetry at mercury electrode.At the surface of mercury electrode,the Yb-TPPS complex is adsorbed by the porphyrin ring,and the ytterbium ion is sitting over the porphyrin plane.The centers of adsorption and the redox reaction for the Yb-TPPS complex are all dependent on the porphyrin ring.The Yb³⁺ ions do not take part in the electrochemical processes.After reduction,the ytterbium porphyrin complex is very unstable and disintegrates completely.

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REACTIONS IN MICROEMULSION FORMED BY ANIONIC－NONIONIC MIXED SURFACTANT,WATER AND HEPTANE

Ji Ming MA, Hu Min CHENG, Zhen Guo ZHAO, Li Min QI

中国化学快报. 1995, 6(01): 67-70.

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The oxidation of iodide by persulfate was studied in the w/o microemulsion formed by mixture of anionic(AOT) and nonionic(NP-6) surfactant,water and heptane.The reaction rate is appreciably higher in a microemulsion formed solely by AOT than that in a conventional aqueous medium.The incorporation of nonionic surfactant deteriorates the catalytic effect of the microemulsion.

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STUDIES OF POLYMER IMMOBILIZED Pd－Cu CLUSTER CATALYSTS PREPARED BY METAL ATOM SYNTHESIS(MVS)

Shi Hua wu, Chang Ying ZHU, Ji Liang ZHU, Xi Sheng SHENG

中国化学快报. 1995, 6(01): 71-74.

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Metal atoms of Pd and Cu produced by coevaporation in a metal atom reactor was solvated at low temperature.These solvated metal atoms were immobilized in the polymer pore structure for preparing Pd-Cu bimetallic cluster catalyst.XPS measurements showed that both Pd and Cu were in a zero-valent state.TEM and XRD results indicated that the Pd-Cu cluster particles were very small.Catalytic tests showed that these catalysts are very active for 4-methyl-3-penten-2-one hydrogenation.

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SELF SUSTAINED SURFACE CHEMICAL OSCHLATION AND IT'S MATHEMATICAL SIMULATION OF THE COMPLETE OXIDATION OF MATHANOL OVER Pt/Al₂O₃ CATALYST

Cong Qi XU, Xiu Yin LIU, Xue Mci WANG, Shu Qing ZHOU, Guo Lin HAN, Ren You ZHNAG

中国化学快报. 1995, 6(01): 75-78.

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A systematic method for studying the self-sustained surface chemical oscillation of the gas-solid catalytic reaction is suggested in this paper.It includcs:(1) the technique of constant temperature,TP-TR,S-TR,(2) the proposed mechanism of the reaction,(3)the mathematical simulation of the reaction and self-susatained surface chemical oscillation.The computed curves coincide with the experimental ones.This result shows that the systematic methods suggested in this paper is feasible.

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STUDY ON XPS,ESR AND MOSSBAUER SPECTRA OF FEZSM-5 WITH ADSORBED ETHYLBENZENE

QiU Bin KAN, Zhi Yun WU, Ru Ren XU

中国化学快报. 1995, 6(01): 79-82.

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XPS,ESR and Mossbauer spectroscopic investigations of iron in Fe-ZSM-5 zeolite show an interaction between adsorbed ethylbenzene(EB) and Fe(Ⅲ) in framework of the zeolite,which causes changes of Fe(2P) binding energy,Mossbauer parameters and ESR signal of framework Fe(Ⅲ) in the zeolite and should be responsible for high catalytic activity of ethylbenzene dehydrogenation over FeZSM-5 catalysts.

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THE CORRELATION BETWEEN ZrO₂ PHASE AND ITS CATALYTIC PROPERTY

Wen LI, Xin Mei WANG, Yuan Qi YIN

中国化学快报. 1995, 6(01): 83-86.

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In this letter,the preparation of three ZrO₂ phases has been briefly described and their catalytic results have been presented for CO hydrogenation to olefin.These catalysts had a good selectivity for light olefin.Monoclinic ZrO₂ catalyst had a high selectivity for isobutene,while the other phase catalysts had not.

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CRYSTAL AND MOLECULAR STRUCTURE OF THE COMPLEX OF METHOXYCARBONYLETHYLTIN TRICHLORIDE WITH SALICYLIDENE－M－TOLUIDINE

Fang Xin FU, Xiu Juan LI, Hua De PAN, Yan XING, Yong Hua LIN

中国化学快报. 1995, 6(01): 87-90.

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The synthesis and properties of the title complex CH₃OCOCH₂CH₂SnCl₃·2-HOC₆H₄CH=NC₆H₄-3'-CH₃ are described.It crystallizes from benzene in the monoclinic space group P2_1/n with unit cell dimensions a=10.326(3),b=6.815(8),c=12.931(6) Å,β=111.52(3)°,V=2088.7(1)Å ³,Z=4,F(000)=1040,μ=16.31 cm^-1,Dc=l.67g/cm³ final R factor is 0.037 for 3177 observed reflections,I≥3σ( I_o).The tin atom in the structure of the complex exists in a distored octahedral geometry defined by three Cl atoms,the C and O atoms of a chelating methoxycarbonylethyl group as well as an O atom derived from the Schiff base ligand.

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SYNTHESIS AND STRUCTURE OF A NOVEL “BUTTERFLY”CLUSTER“MoOS₃Cu₂(Py)₂(PPh₃)₂”

Hong Wei HOU, Xin Quan XIN, Xiao Xing HUANG, Jin Hua CAI, Bei Sheng KANG

中国化学快报. 1995, 6(01): 91-92.

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Reactions of [NH₄]₂MoO₂S₂,CuI and PPh₃ in Py produced mixed-metal cluster [MoOS₃Cu₂(Py)₂(PPh₃)₂],which crystallizes in the monoclinic,space group P2₁/a with a=18.149(4),b=10.044(3),c=25.171(7)Å,β=107.45(2) °,V=4377(2)Å³,Z=4,D_x=1.54,R=0.040,R_w=0.049.The results of structure determination show that the central unit of the cluster compound is composed of three metal and three sulfur atoms.

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VARIATION OF C₆₀ SOLUBILITY WITH TEMPERATURE

Yong Jun LENG, Wan Xi CHEN, Zhu De XU, Wen Zhu LI

中国化学快报. 1995, 6(01): 93-94.

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Abstract Temperature dependence of C₆₀ solubility in four organic solvents above room temperature was investigated.It is found that the solubilities decrease with increase in temperature in hexane,toluene and xylene while it increases in cyclohexanc.Least square fit gives the heat of solution of C₆₀ in hexane,toluene,xylene and cyclohexane as-6.0,-9.8,-9.1 and 48.2 KJ/mol respectively.

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1995年, 第6卷, 第01期　刊出日期：1995-01-20

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1995年, 第6卷, 第01期 刊出日期：1995-01-20

1995年, 第6卷, 第01期　刊出日期：1995-01-20