中国化学快报

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A NEW SULFINATODEHALOGENATION REAGENT:THIOUREA DIOXIDE

Wei Yuan HUANG, Jin Lian ZHUANG

中国化学快报. 1990, 1(03): 191-192.

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The reaction of perfluoroalkyliodides, perfluoroalkylbromide, 1, 1, 1-trifluoro-2, 2, 2-trichloro-ethane, and carbon tetrachloride with thiourea dioxide in aqueous acetonitrile solution gave the corresponding sulfinate in good yield.

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STUDIES ON THE REACTION OF SULFUR, SELENIUM AND TELLURIUM WITH SODIUM HYDROXIDE UNDER PHASE TRANSFER CATALYSIS(Ⅱ).A CONVENIENT METHOD FOR THE SYNTHESIS OF BI(ACYL)DISULFIDES

Jin-Xian WANG, Chin-Hsien WANG, Wen feng CUI, Yu lai HU, Kai ZHAO

中国化学快报. 1990, 1(03): 193-196.

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A simple and general method for the synthesis of bi(acyl)disulfides isreported.Sulfur is allowed to react with sodium hydroxide to give sodium disulfideat 65℃ under PTC, which can react with acyl halides to afford bi(acyl)disulfides ingood to excellent isolated yields.The effects of solvents and phase transfercatalysts are discussed.

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AN INVESTIGATION ON THE INTERACTION MECHANISM OF β-CAROTENE WITH HALOGEN ATOM PRODUCED IN HALOBENZENE BY UV IRRADIATION

Yong LI, Bing SHI, Qing Gui SHA

中国化学快报. 1990, 1(03): 197-200.

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ESR measurements using spin trapping technique were carried out for β-carotene-halobenzene system under UV light irradiation.The ESR spectra observed in the presence and in the absence of β-carotene are markedly different.Thepossible scheme of β-carotene interacting with halogen atom was proposed.

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PHOTOINDUCED ELECTRON TRANSFER I.INTER-AND INTRAMOLECULAR QUENCHING OF ZINC PHTHALOCYANINE FLUORESCENCE BY ANTHRAQUINONE

Shu Yin SHEN, Li LI, Qing Fu ZHOU, Hui Jun XU, He Zhou WANG

中国化学快报. 1990, 1(03): 201-204.

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Inter-and intramolecular quenching of zinc phthalocyanine fluorescence by anthraquinone has been studied.The diminutions of fluorescence quantum yield and life-time are due primarily to electron transfer.Apparent electron transfer rate constants were calculated depending on the chain length and solvent polarity.

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SYNTHESIS OF 2, 3-SUBSTITUTED QUI NOXALINE FROM α-KETOTHI OANI LI DE

Zhong E LU, Le Cun XU

中国化学快报. 1990, 1(03): 205-206.

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A method of synthesis of quinoxaline by α-ketothioanilide and o-phenylenediamine is described in this paper.

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SYNTHESIS OF(4S, 5R)-5-HYDROXY-4-DECANOLIDE.THE PROPOSED AUTOREGULATOR FROM STREPTOMYCES

Da Qing SUN, Ke Qian CHEN

中国化学快报. 1990, 1(03): 207-208.

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(4S, 5R)-5-Hydroxy-4-decanolide 1, the proposed autoregulator from streptomyces Griseus was synthesized from an allyl alcohol 2, employ-ing the Sharpless kinetic resolution and the reaction of diethyl malonate with the epoxy compound 4 as two key steps.

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A NEW ONE-STEP REDUCTIVE N-ALKYLATION OF AMINO ACIDS AND THEIR ESTERS

De Ling Zhou, Ye Di Guan, Sheng Jin

中国化学快报. 1990, 1(03): 209-210.

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The reductive alkylation of amine with carbonyl compounds using sodium hydrogen telluride has been investigated in recent years⁽¹⁾.Application of this method to the synthesis of N-alkyl derivatives of biologically important amino acids and their esters is described.

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A FACILE SYNTHESIS OF 2-AND 2, 4-UNSATURATED AMIDES

Qi ZHONG, Chang Qing LIU

中国化学快报. 1990, 1(03): 211-212.

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A convenient method for preparing unsaturated amides via telluro-nium salts employing solid potassium carbonate as a base with high stereo-selectivity in excellent yields has been developed.

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STUDIES ON GLYCOSIDES Ⅷ.TOTAL SYNTHESIS OF NEW ALKALOID GLYCOSIDES FROM SELAGINELLA DOEDERIENⅡ

Zhan Jiang LI, Cheng Fang YU, Meng Shen CAI

中国化学快报. 1990, 1(03): 213-214.

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Two new alkaloids, hordenine-O-α-L-rhamnopyranoside(Ⅰ)and hordenine-0-(6"-trans-cinnamoyl)-4'-O-β-D-glucopyranosyl-α-L-rhamnopyranoside (Ⅲ) isolated from Selaginella doederleinii have been synthesized the first time.A new method, in which trifluoroacetoxyl group was used both as a good leaving group and a protecting group for synthesis of O-glycosides with high stereo-selectivity was reported.

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SYNTHESIS OF 5α-(17R, 20R)-14, 15-SECOCHOLESTANE

Tong Shuang LI, Yu Lin LI, Xiao Tian LIANG

中国化学快报. 1990, 1(03): 215-218.

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The synthesis of 5α-(17R, 20R)-14, 15-secocholestane from cholesterol was reported.

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CHEMICAL CONSTITUENTS OF LONICERA MACRANTHOIDES HAND.-MAZZ Ⅰ.STRUCTURE OF MACRANTHOISIDE I

Min CHEN, Si Qi LUO, Hui Ting LI

中国化学快报. 1990, 1(03): 219-220.

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A new bisdesmosidic triterpene saponin, macranthoiside I, was isolated from L.macranthoides.Its structure was determined by chemical degradation and spectroscopic analysis.

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APPLICATION OF 2D-NMR TECHNIQUES IN THE STRUCTURE DETERMINATION OF HYPODEMATINE

Ya Min CHEN, Ying Hua LU, Yan Jun CHEN, Cun Sheng MA, De Quan YU

中国化学快报. 1990, 1(03): 221-222.

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An alkaloid with a novel structure, named Hypodematine, was isolated from Hypodematium sinense Iwatsuki(belonging to Thelypterdaceae)⁽¹⁾.Its structure was elucidated by means of the ¹H-¹H COSY' ¹H-¹³C COSY and long-range ¹H-¹³C COSY spectroscopy to have the skeleton of benzo-aza-cyclooctatetraene with a phenyl substituent.Such basic structure has not been found in the na-tural product before.

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STRUCTURE OF VERSICOLACTONE A, A NOVEL SESQUITERPENE LACTONE FROM ARISTOLOCHIA VERSICOLAR S.M.HWANG

Jiu ZHANG, Lin Xing HE, Hui Zhong XUE, Rui FENG

中国化学快报. 1990, 1(03): 223-224.

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A novel sesquiterpene tactone, versicolactone A, with 12-carbon ring skeleton, has been isolated from the roots of Aristolochia versicolar S.M.Hwang, and the structure was elucidated on the basis of 2D NMR and MS spectral data.

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GC-MS STUDY ON DIURETICS IN URINE Ⅰ.BETECTION METHOD USING METHYLATION

Ya wei LI, Jun LI, Shao Tang ZHU, Tong Hui ZHOU

中国化学快报. 1990, 1(03): 225-228.

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A reliable and sensitive method is developed for the detection of common diuretics in human urine. diuretics along with probenecid are methylated and subjected to GC-MS analysis.Both chromatographic and mass spectrometric data are obtained in selected ion monitoring and full scanning modes.The average detection limit is 0.1-1.0 ug/mi urine.This method is suitable to large-scale and routine screening or confirmation of diuretics in doping control.

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HIGHLY SENSITIVE SPECTROPHOTOMETRY OF NIOBIUM

Zong Ming LUO

中国化学快报. 1990, 1(03): 229-230.

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In pH2.0-3.0, niobium(V) forms molybdonlobic acid with sodium molybdate.A spectrophotometric method has been developed for the deter-mination of niobium based on the formation of ion-associate compound of molybdoniobate with Butyl Rhodamine B in aqueous solution in the presence of polyvinyl alcohol and 0.4-0.7 mol/L H₂SO₄.The maximum absorption of ion-associate compound exhioits at 85 nm and the molar absorptivity is 7.5×1.0⁵ L.mol^-1.cm^-1for niobium.The new method has been applied to the determination of microamounts niobium in silicate rock, when niobium content is at the level of 8×10^-3%, with the relative standard deviation of about 3%.

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Analysis of Beta-blockers in Doping Control

Hong Jin DUAN, Hong Ju FANG, Yan Qing XU, Tong Hui ZHOU, Hua CHI, Yun WU, You Xuan XU

中国化学快报. 1990, 1(03): 231-234.

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A retiabte and sensitive method is developed for the detection of β-blockers which are excreted in free or conjugated forms in human urine.9 β-blockers were derivatized by MSTFA and MBTFA and subjected to GC/MSB analysis.Both chromato-grams and mass spectrometric data were obtained from full scanning mode.This method is suitable for routine screening and confirmation of β-blockers in doping control.

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ON-LINE ELECTROLYTIC DISSOLUTION OF SOLID METAL SAMPLE AND DETERMINATION OF COPPER IN ALLOY BY AAS

Dong Xiang YUAN, Peng Yuan YANG, Xiao Ru WANG, Ben LI HUANG

中国化学快报. 1990, 1(03): 235-236.

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On-line dissolution of solid metal sample can be carried out by electrolysis under the control of flow injection analyzer(FIA), and the dissolved sample can be transferred to atomic spectrometer for the direct analysis.The hyphenated technique of FIA on-line electrolytic dissolution of alloy and atomic absorption spectrometer (AAS) detection is developed.The research is focused on the effects of electrolyte composition and electrolysis parameters on the sample dissolving, as well as the quantitative analysis of Cu in Al alloy samples.

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PRECONCENTRATION OF TRACE ZINC IN SEAWATER ON CPPI RESIN BY FIA AND ON-LINE DETECTION BY ICP-AFS

Dong Xing YUAN Peng Yuan YANG Xiao Ru WANG Ben Li HUANG

中国化学快报. 1990, 1(03): 237-238.

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A quite new type of chelating resin Carboxymethylated Polyethylenimine-Polymethylenepolyphenylene Isocyanate (CPPI) is use dfor the preconcentration of Zn from high salt water such as seawater.The preconcentration is controlled through the technique of Flow Injection Analysis(FIA).The concentrated sample solution is then directly transferred to an Inductively Coupled Plasma-Atomic Fluorescence Spectrometer(ICP-AFS)for determination.The detection limit of Zn by the technique is about 0.06 ppb.

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POLAROGRAPHIC CHARACTERISTICS OF TELLURIUM(Ⅳ) IN ALKALINE DYE-ACID SOLUTION

Li Hua ZHU, He Qing TANG, Wen Zhao SHI

中国化学快报. 1990, 1(03): 239-240.

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Polarographic characteristics of Te(Ⅳ)-alkaline dye were investiga-ted at mercury electrode in acidic solution.It was found that the mechanism of the electrode process depended on the concentration of Te(Ⅳ).

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ORGANIC NONLINEAR OPTICAL CRYSTAL:N-(4-NITROPHENYL)-(s)-(+)-2-PYRROLIDINEMETHYLENE TOSYLATE(NPP-OTs)

Cheng YE, Nai Jue ZHU, Mei Xiang WAN, Yan LI

中国化学快报. 1990, 1(03): 241-244.

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Large crystal NPP-OTs has been obtained by growth from solution, its powder SHG efficiency is 1/3 of urea.It shows it is a new convenient approach to obtain organic second-order NLO crystal:the dipole-dipole interaction is oppos-ed by introducing a large side group.

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MOLECULAR AND CRYSTAL STRUCTURES OF TETRANUCLEAR MOLYBDENUM CLUSTER[MO₄(μ3-O)₂O₄Cl2(o-CH₃C₆H₄COO)⁶]

Zhong Sheng JIN, Ge Cheng WEI, Yung Shing LIU, Gang DONG, Chun Ting SUN, Qi Jun HUANG, Fan YANG

中国化学快报. 1990, 1(03): 245-246.

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The new cluster[MO₄(μ3-O)₂O₄Cl2(o-CH₃C₆H₄COO)⁶]has been prepared by the reaction of molybdenum pentachloride and o-methylbenzoic acid.The crystal and molecular structures were determined by the X-ray diffraction method.It crystallizes in the orthorhombic space group Pnna with cell parameters:Mr=1361.6, a=13.792(4), b=17.957(3), c=20.974(9)Å , V=5194(2) 3, Z=4, Dc=1.74/cm³, F(OOO)=2704, μ(MoKα)=11.0/cm, R=0.074.

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RAPID DETERMINATION OF PROTEIN IN MILLET BY FOURIER TRANSFORM NEAR-INFRARED (FTNIR) DIFFUSE REFLECTANCE SPECTROSCOPY

Le Ming SHI, Zhi Hong XU, Zhong Xiao PAN, Zhi Liang LI, Yan Lu YAN, Mao JIN

中国化学快报. 1990, 1(03): 247-250.

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In this paper, the Fourier transform near-infrared (FTNIR) diffuse reflectance spectroscopy is applied for the rapid determination of protein in millet.The partial least-squares (PLS) regression is successfully used as an effective multivariate calibration technique.The calibration set is composed of 20 standard millet samples that the protein contents were determined by the traditional Kjeldahl method.The optimal model dimension is found to be 5 by cross-validation.22 millet samples were determined by the proposed FTNIR-PLS method.The correlation coefficient between the concentration values obtained by the FTNIR-PLS method and the traditional Kjeldahl method is 0.9805.The standard error of prediction (SEP) is 0.28% and the mean recovery is 100.2%.The proposed method has been successfully applied for the routine analysis of protein in about 10,000 grain samples.

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A SPECTROPHOTOMETRIC STUDY OF THE COMPLEXATION EQUILIBRIUM OF IRON(Ⅱ)WITH 4-(2-THIAZOLYAZO)-RESORCINOL

Ke An LI, Feng LIU, Tao ZHU, Shen Yang TONG

中国化学快报. 1990, 1(03): 251-254.

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4-(2-thiazolyazo)-resorcinol(TAR)can form complexes FeR, FeHR and FeR2 according to numerical evaluation from experimental data of A and pH.Their cumulative stability constants(log B)are 11.48, 15.32 and 17.30 respectively.

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SYNTHESIS AND CRYSTAL STRUCTURE OF A ONE-DIMENSIONAL POLYMERIC CLUSTER[Mo(μ-S)2Ag(μ-S)2·α-MePyH]n

Ji Guo LI, Xin Quan XIN, Zhong Yuan ZHOU, Kai Bei YU, Li LIU

中国化学快报. 1990, 1(03): 255-256.

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Reaction of (NH₄)₂MoS₄ with AgI in α-MePy gives the title com-pound, an X-ray analysis of which shows that the molecule forms a one-dimensional polymeric chain with continuous metal-metal bonds.

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FRACTALS OF HYBRID ORBITALS AND THEIR APPLICATIONS IN THE ENZYME MODELS

Hou Qiang LI, Shu Hua CHEN, Hua Ming ZHAO

中国化学快报. 1990, 1(03): 257-260.

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An enzyme is a kind of protein with catalytic activity and long chain, and its structure and shape are determined by the hybridized state of atomic orbital.The fractal dimension (D_f) is closely related to the hybridization, e.g.D_f=2ln2/ln[2(1+α/(1-α))]for the sp^a type, where a denotes the fraction of the s orbital in the hybridized molecular orbital.This relationship and the five fractal theorems introduced by the present paper play an important role in the investigations of the model of imitative enzyme.

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A STUDY OF PHOTOELECTROCHEMICAL CELLS BASED ON SILICON ELECTRODES COATED WITH METAL LAYERS

Huai Xiang Li, Shi Xun Wang, Guo Zheng Li

中国化学快报. 1990, 1(03): 261-262.

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Photoelectrochemicat cells, composed of different epitaxial n-Si photoele trodes coated with metal such as nickel o platinum and immersed in a solution of redox couple Br Br₂ or Fe(CN)6^4-/3-, are investigated.A high conversion efficiency from optical to electri-cal energy up to 13.6% can be achieved under optimum conditions.

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THE SYNTHESIS AND CHARACTERIZATION OF THE COORDINATION COMPOUNDS OF Pt(Ⅱ) AND Ir(Ⅲ) WITH 2-MERCAPTOPYRIDINE-1-OXIDE AND ITS METHYL DERIVATIVES

Bao Lin SONG, Yang CAO, De Zhong NIU, Zai Sheng LU, Cheng ZENG

中国化学快报. 1990, 1(03): 263-264.

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Six coordination compounds of Pt(Ⅱ)L₂ and Ir(Ⅲ)L3 type(where L is PT^-, 3Me-PT^- or 4Me-PT^-) are reported here.Four coordination compounds of the latter two ligands have never been reported before, while PT^-'s were synthesized with H₂PtCl₆ and (NH₄)3IrCl₆ respectively, which were different from the methods of Davidson et al.¹ and Sterinbrec H².They were characterized by elemental analysis, UV, IR, ¹HNMR and molar conductance.Their structural formulas have beendetermined, and the mechanism of synthetic reaction has been discussed.

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NON-ACETAL INITIATORS FOR GROUP TRANSFER POLYMERIZATION

You Si ZOU, Hai Ping XIA, Rong Hua PAN

中国化学快报. 1990, 1(03): 265-268.

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It is reported that a variety of trimethylsilyl enol ethers of ketones and aldehydes can be used to initiate GTP of methacrylates and acryl-ates.The new initiators are easy to prepare from ketones or aldehydes.PMMA and PMA with controlled molecular weight and low polydispersity were obtained by using non-acetal initiators in the presence of bibenzoate, bifluo ide or Hgl₂, The living nature of polymerization is shown by the correspondence of theoretical and observed molecular weight and the preparation of A-B-A type triblock copolymer with methacrylate and acrylate segments can be prepared.

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REMOVAL OF ORGANIC POLLUTANTS USING TITANIUM DIOXIDE MEDIATED PHOTOCATALYTIC OXIDATION

Man ping ZHANG, Zong feng XIA, Shinan XIE, Pei pei LI, Junbo BAO, Ju ying WANG, Daiwen KANG, Yujun WANG, Nian hong CHEN, Li dong YU, G. K-C LOW

中国化学快报. 1990, 1(03): 269-270.

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A simple and effective method of removing polluted organics in water is reported here.Titanium dioxide is a catalyst in photo-oxidation of monocrotophos.The mechanism of photocatalytic oxidation and the kinetics of the reaction were studied.This same principle also leads to the construction of instrument of PTR-FIA analysis for monitoring organic phosphorus and phosphate in water.

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NONLINEAR OPTICAL PROPERTY OF para-DISUBSTITUTED BENZYLIDENE-ANILINE DERIVATIVES

Daoyu LIU, Chaoyang DAI, Jingui QIN, Xiaoping GONG, Chuang tian CHEN, Bai chang WU

中国化学快报. 1990, 1(03): 271-274.

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Forty para-disubstituted benzylidene-aniline derivatives were synthesized, and their second harmonic generation (SHG) efficiency was measured by the Kurtz powder technique.The effect of the electronic property and the position of the substituents on powder SHG efficiency was studied.

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SEMICONDUCTING PROPERTIES OF In2O₃ ANODIC FILM

Zhong hua LIN, Hai yi CHEN, Zhaowu TIAN

中国化学快报. 1990, 1(03): 275-276.

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The good potentiality of the In2O₃ anodic film as a photoanodic material has been demonstrated.The anodic oxidation of In substrate in alkaline solution for obtaining In₂O₃ film has been developed and their semiconducting properties have been investigated through capacitance, photoelectrochemistry and electroreflection measurements.

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PREPARATION OF FINE α-AL₂O₃ BY THERMAL DECOMPOSITION OF HYDRAZINE-CONTAINING ALUMINUM SALT

Jie Da WU, Guang Rong YANG

中国化学快报. 1990, 1(03): 277-278.

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A new method for preparing fine α-Al₂O₃ by thermal decomposition from hydrazine-containing aluminum salt was described.The process of the thermal decomposition of the hydrazine-containing aluminum salt was investigated by thermal analysis (TG and DTA) and the thermally decomposed products were studied by S.E.M and X-ray diffraction.The result indicated the particles of α-Al₂O₃ obtained in this way at 12500℃ were < 1μm in size.

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SINERING BEHAVIOUR OF RANEY-COPPER CATALYST IN VARIOUS ATMOSPHERES

Chong Zheng FAN, Chang Sui WANG, Sheng Jun WANG, You Shi WU, D. L. TRIMM, M. S. WAINWRIGHT

中国化学快报. 1990, 1(03): 279-282.

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Raney-Copper (R-Cu) catalyst was prepared and its sintering behaviour in atmospheres at teperature 300℃-600℃ was detected by methods of SSA, PSD, XRD and SEM.It was found that sintering of R-Cu started from much lower temperature than the melting point of copper.Changes both on the surface and in the body phase were discovered.There is a rule in the extent of sintering for R-Cu in different atmospheres which is related to the adsorption of the particular gases molecules on the surface of the catalyst.Dynamical equations of the surface decrease is established and the mechanism of sintering is discussed.Calculations of quantum mechanics givethe similar results.

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EFFECT OF HYDRATION ON THE THERMAL STABILITY OF ENZYME

Yun Na LIU, Fu TAN

中国化学快报. 1990, 1(03): 283-284.

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The thermal stability of New Zealand culture rabbit muscle aldolase was investigated by differential scanning calorimetry in the water content range 0.23-3.70 g water per g protein.The experimental results showed that at water contents below 0.47g/g, an endothermic peak was observed and at water contents above 0.57g/g, an endothermic and an exothermic peak were both observed on DSC thermogram.Thermal denaturation result of the enzyme and the relationship between two transition temperatures and water contents were first reported in this paper.Up to now we have not seen any similar reports concerning the exothermic transition.

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1990年, 第1卷, 第03期　刊出日期：1990-12-20

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1990年, 第1卷, 第03期 刊出日期：1990-12-20

1990年, 第1卷, 第03期　刊出日期：1990-12-20