中国化学快报

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STUDIES ON THE PRENYLFLAVONOIDS PART Ⅲ⁽¹⁾.SYNTHESIS OF(±)EUCHRENONE A⁸

Hua Wu SHAO, Fang Jie ZHANG, Yu Lin LI

中国化学快报. 1993, 4(03): 189-190.

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(±)Euchrenonc a8,7,2'-dihydroxy-8,5'-di(γ,γ-dimethylallyl)-4'-methoxyflavanone,has been synthesized by the condensation of 2-hydroxy-4-methoxymethoxy-3-(γ,γ-dimethylallyl)acctophenonc with 4-methoxy-2-methoxymethoxy-5-(γ,γ-dimethylallyl)benzaldchyde followed by cyclization and demethoxymethylation.

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SYNTHESIS OF 3-METHOXYCARBONYL -4-METHL-9-AZABICYCLO[4.2.1] NON-3-ENE AND 3-ACETYL-4-METHYL-9-AZABICYCLO[4.2.1]NON-3-ENE

Hong Chun TANG, Dao Xiao HUANG, Yu Lin LI, Xu Bao DU, Hong Shou LIAN, Ji Sheng CHEN

中国化学快报. 1993, 4(03): 191-194.

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New bicyclic alkaloids. 3-methoxycarbonyl-4-methyl-9-azabicyclo[4.2.1]non-3-ene(Ⅱ)and 3-acetyl-4-methyl-9-azabicyclo[4.2.1]non-3-ene(Ⅲ).have been synthesized from tropinone through eight and ten steps.respectively.The key features of the synthsis are the cuprate coupling reaction of acyclic enol phpsphates at lower temperatures to achieve high stereoselectivity and de-N-methylation with 2,2,2-trichloroethoethoxycarhonyl chloride proceeded smoothly.

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STEREOSELECTIVE SYNTHESIS OF SUBSTITUTED(PYRIMIDIN-2-YL)1-THIOGLYCOPYRANOSIDES

Jian Xin YU, Fang Min LIU, Xiao Jun CI, Ling Hua CAO

中国化学快报. 1993, 4(03): 195-196.

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The polyacetylated(4,6-dimethylpyrimidin-2-yl)1-thioglycopyrano-sides(5-8) were obtained in high yields with stereoselectivity by phase-transfercatalyzed synthesis,and their structures were confirmed by elemental analysisand IR,¹H-NMR spectral data.

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STUDIES ON THE SYNTHESIS OF D-GLUCURONIC ACID DERIVATIVES OF 2-BUTOXY-5-FLUORO-3H-4-PYRIMIDONE AND THEIR ANTICANCER ACTIVITIES

Chang Jun SUN, Zai Cheng CHEN, Yi Gui WAN,G Peng XUE, Feng Yao LIU

中国化学快报. 1993, 4(03): 197-198.

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2-Butoxy-5-fluoro-3H-4-pyrimidone derivatives of D-glucuronic acid having 0-glycosidic linkage or N-glycosidic linkage were synthesized and their anticancer activity tested.Their structures were confirmed by elementary analysis,IR spectraand ¹HNMR.

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SYNTHESIS,PHOTOCHROMIC PROPERTIES OF PYRRYL SUBSTITUTED HETEROCYCLIC FULGIDES

Lian He YU, Yang Fu MING, Mei Gong FAN

中国化学快报. 1993, 4(03): 199-202.

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Nine new 3-acetyl pyrrole derivatives and corresponding 3-pyrryl substituted heterocyclic fulgides:3-pyrryl-ethylidene(isopropylidene)succinic anhydrides have been synthesized and characterized.Their photochromic behavour in several organic solvents were investigated.The coloured form of fulgide Ⅱc,(E)-α-(1,2,4-trimethyl-3-pyrryl)-ethylidene(isopropylidene)succinic anhydride,shows absorption maxmium at 715nm in acetonitrile.It is the longest absorption among the known photochromic fulgides

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USE OF CATION EXCHANGE RESIN IN SYNTHESIS OF N-SUBSTITUTED-1-AMINOALKANEPHOSPHONATE AND-PHOSPHINIC ACIDS

Yue Hua ZHANG, Wen Qiang HUANG, Ai Ju MEN, Bing Lin HE

中国化学快报. 1993, 4(03): 203-204.

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Strongly acidic cation exchange resin(001x1,H form)has been successfully used as a catalyst in synthesis of diphenyl N-benzyloxycarbonyl-1-aminobenzylphosphonate,N-benzyloxycarbonyl-1-aminobenzylphenylphosphinic acid and N-p-tolylsulfonyl-1-aminobenzyl phenylphosphinic acid in high yields.

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SYNTHESIS AND PHASE BEHAVIOR OF LIQUID CRYSTALLINE 4'-ALKYLOXY-4-HYDROXYBIPHENYLS

Jing LIN Liang, Tan CHEN, Qing Qing YAO, Hai Shui HUANC

中国化学快报. 1993, 4(03): 205-208.

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The synthesis and phase behavior of a series of 4'-alkyloxy-4-hydroxy biphenyls were discribed.The effects of reaction conditions on the yields of products were investigated.The characterizations of thermotropic liquid crystalline products for the type and thermal properties are discussed through the use of differential scanning calorimetry,polarizing microscopy.

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RE-DISTRIBUTION OF THE N-METHYL GROUP IN GELSEMINE

Guo Feng HUANG, Fang SUN, Zong Ping ZHANG, Xiao Tian LIANG, Qi Yi XING

中国化学快报. 1993, 4(03): 209-212.

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The N_(b)-bromomethyl derivative (2) of gelsemine,a quaternary ammonium salt,was found to be recalcitrant toward Hofmann type alkaline degradation which has been successful in other cases.Instead,a re-distribution of the N-methyl group took place,giving rise to 3a,1,3b and 3c,in descending order of Rf values.

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THE STUDY ON THE WATER SOLUBLE PEPTIDES IN PAPAVER SOMNIFERUM POLLEN EXTRACTION,PURIFICATION,SEQUENCE DETERMINATION AND SYNTHESIS

Jia Xi XU, Sheng JIN

中国化学快报. 1993, 4(03): 213-214.

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Four peptides PSPP1,PSPP2,PSPP3 and PSPP4 were purified from the water-extractof Papaver somniferum pollen.Their sequences,with 21,17,13 and 16 amino acid residues respectively,have been determined by Edman degradation-N-terminal dansylation.PSPP2,PSPP3 and PSPP4 were synthesized using solid phase method.The immunopromotive activities of PSPP1,PSPP2,PSPP3,PSPP4 and the initially separated sample PSPP have been also observed by the methods of counting erythrocyte rosette forming cells(ERFC) and T-lymphocyte transformation test in vitro.

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THEORETICAL STUDY ON PHOTODECARBONYLATION REACTION OF ACROLEIN

Wei Hai FANG, Ming Bao HUANG, De Cai FANG, Ruo Zhuang LIU

中国化学快报. 1993, 4(03): 215-216.

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Photodecarbonylation reaction of acrolein at 193nm was investigated by ab initio molecular orbital method.Our result supports photodecarbonylation mechanisms proposed by Fujimoto,and predicts that the reaction should occur in ⁸ππ^* potentialenergy surface prior to the ¹ππ^* potential energy surface.

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REACTIONS OF ORGANODILITHIUM COMPOUND WITH ALKYL HALIDES

Zhen Wei HUAN, Wei Guo LIU, Ling Jun BAI

中国化学快报. 1993, 4(03): 217-218.

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The mechanism of the electron transfer reaction of 1,4-dilithio-tetraphenyl-1,3-butadiene with methyl iodide was studied.

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A NEW ALKALOID FROM CELASTRUS ANGULATUS

Yong Qiang TU, Yu Xin CUI, Yong Xiang MA

中国化学快报. 1993, 4(03): 219-220.

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A new β-dihydroagarofuran alkaloid Ⅰ was isolated from Celastrus angulatus.The structure was established on the basis of 1D and 2D NMR analysis,and x-ray diffraction.

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STUDIES ON THE PROPERTIES OF SCHIFF BASE TYPE ARYLMERCURY COMPOUNDS Ⅲ TRANSMETALLATION REACTION OF SCHIFF BASE TYPE ARYLMERCURY COMPOUNDS WITH METALLIC TIN

Kui Ling DING, Yang Jie Wu, Yang WANG, Li YANG

中国化学快报. 1993, 4(03): 221-224.

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The transmetallation reaction of 4 Schiff base type arylmercury compounds with metallic tin has been carried out in refluxing xylene.It was found that the reaction proceeds in the same manner as that of chloro[2-(phenylazo)phenyl]mercury(Ⅱ)to give dichlorobisaryltin(Ⅳ).The ¹H NMR spectra of the products provide evidence for the presence of N→Sn intramolecular coordination.The formation of dichlorobisaryltin(Ⅳ)as a unique product probably arises from the N→Sn intramolecular coordination which results in the increasing of the stability of the molecule.

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THE SYNTHESIS AND CHARACTERIZATION OF ANSYMMETRIC PENTAAZADENTATE PORPHYRIN-LIKE METAL COMPLEXES^*

Wen Fang SUN, Duo Yuan WANG

中国化学快报. 1993, 4(03): 225-228.

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This paper presents the synthesis and structural characterization of asymmetric tripyrrane-containing macrocycle.This macrocycle could be oxidized to the methine bridged,22 π-electron aromatic macrocyclic complexes containing cadmium(Ⅱ),samarium (Ⅲ),europium(Ⅲ)and gadolinium(Ⅲ)by treating with corresponding metal chloride in the presence of air Their structures were characterized by spectral methods.

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CHROMATOGRAPHIC SEPARATION ON GRAPHITE OF FULLERENE-C₆₀ AND-C₇₀

Ling ZHU, Han Yao LIANG, Su Nian CHEN, Rong Sheng SHENG

中国化学快报. 1993, 4(03): 229-232.

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The mixture of fullerene—C₆₀ and —C₇₀ was successfully separated in larger amount by liquid chromatography on graphite column.The column was first eluted with a mixture of hexane and toluene,and then with toluene.The eluates were monitored by UV/visible absorption spectroscopy.Graphite column shows high performance for separation.and much larger quantities of pure C₆₀ can be easily obtained.The synthesis of fullerenes(C₆₀ and C₇₀)in macroscopic quantities^[1,2] has stimulated scientists to study on themethod for separating C₆₀ and C₇₀.Because of the poor solubility of fullerenes C₆₀/C₇₀ in most organic solvents,theseparation of C₆₀ and C₇₀ proved to be a challenging task.Most attempts at the separation have used silica and alu-mina as the stationary phase and a mixture of hexane and benzene(or toluene)as the mobile phase^[3,5].Fullerenes,however,have only limited solubility in hexane,these separations are usually only achieved by limit-ing the amount of sample to a few milligrams.The hexane-silica technique using phenylglycine based HPLCcolumns appears to offer good separation^[6],but only for submilligram amounts. The use of graphite powder as the stationary phase in liquid chromatography is an advanced separation tech-nique for fullerenes C₆₀/C₇₀^[7,8].The technique is based on that the fullerene-C₆₀ is different from C₆₀ in the de-gree of electron delocalisation,and C₆₀ is much less diamagnetic than C₇₀.It is expected that the dissimilarity willcause the C₆₀/C₇₀ molecules to exhibit different interactions with graphite,and can be separated from each other onthis basis.

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STUDY OF DERIVATIZATION OF PROTEIN WITH A EUROPIUM CHELATE AND APPLICATION TO HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

Xiao Da YANG, Lan HUANG, Qing Wei WANG, Yun Xiang CI

中国化学快报. 1993, 4(03): 233-234.

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A europium chelate of 5-chlorosulfoyl-2-thenoyltrifluoroacetone(CTTA)was investigated for precolumn derivatization ofprotein for high performance liquid chromatography.This new label was highlyfluorescent and suitable for time-resolved fluorometric detection.Thedetective limit of protein is less than 0.3ug in sample with a volume of100ul.Theoretically,the new label can also be used in gel electrophoresisand protein blotting.

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AN IMPROVED NONADIABATIC COLLISION MODEL FOR ION-PIR FORMATION PROCESS:A+BC → A⁺+BC^-

Zheng Ting CAI, Yu Guang MU

中国化学快报. 1993, 4(03): 235-238.

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Hickman's fast nonadiabatic collision model for the ion-pair formation reaction A+BC→A⁺+BC^-was improved,where the classical trajectory has been represented by solution of motion equation UR=-dV(R)/dR,here V(R)is Morse potential.Employing this model to the CS+O₂→CS⁺+O₂^-reaction,a satisfactory agreement with experimental data has been obtained.

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AB INITIO STUDY OF LOW-LYING ELECTRONIC STATES OF THE AsH₂ RADICAL

Zheng Li CAI

中国化学快报. 1993, 4(03): 239-242.

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The equilibrium geometries,excitation energies,force constants and vibrational frequencies for the low-ly-ing electronic states X²B₁,²A₁,²B₂ and ²A² of the AsH₂ radical have been calculated at the MRSDCI level witha 3-21G^* basis set.Our calculated geometries,excitation ene_-gies and vibional frequencies for the X²B₁ and ²A₁ states are in good agreement with available experimental data.The electronic transition dipole moments,oscillator strengths for the ²A₁→X ²B₁ and ²A₂→X ²B₂1 transitions,radiative lifetimes for the ²A₁ and ²A₂ states are calculated based on the MRSDC1 wavefunctions,predicting results in reasonable agreement withavailable experiment.

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THE LINEAR CORRELATIONS BETWEEN ELECTRONIC TRANSITION ENERGY AND HAMMETT CONSTANTS FOR THE SUBSTITUTED PORPHYRIN-LIKE MACROCYCLE

Shi Ming DONG, Duo Yuan WANG

中国化学快报. 1993, 4(03): 243-246.

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The properties of absorption spectra are presented and the linear correlations of Hammett constants with the 0-0 transition energy(Eo,o)of S₁←S^o,and the ratios of oscillator strength(f_a/f_e)are used to probe the interactions betwee π-electron of aromatic maerocycles or metal ion of complexes with the substituents on β-position of benzene ring for porphyrin-like maerocyclic compounds

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A1HNMR STUDY ON THE FORMATION AND BREAKING OF INTRAMOLECULAR HYDROGEN BONDS OF BILIRUBIN IN CDCl₃-DMSO-d₆ BINARY SOLVENT

Qing Xiang GUO, Zi Zhong LI, Jun WANG, You Cheng LIU

中国化学快报. 1993, 4(03): 247-250.

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The formation and breaking of intramolecular hydrogen bonds of bilirubin in CDCl₃-DMSO-d₆ binary solvent have been investigated by means of NMR spectroscopy.The chemical shifts of protons at dipyrrinone lactam C=Oand N-H,Pyrrole N-H,C-5,C-15 and methylene groups of 8,12-propionic acid side-chains changed markedly as a function of composition of the binary solvent.The hydrogen bond formation is dependent on the conformation of propionic acid side-chains.

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EPR STUDY OF THE FORMATION OF[Li⁺O^-]ION PAIR ON Li-DOPED ZnO^t

Ting Lu YANG, Liang Bo FENG, Shi Kong SHEN, Han Qin Wang

中国化学快报. 1993, 4(03): 251-254.

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In this letter the study of Li-doped zinc oxide by electron paramagnetic resonance method is described.A signal observed atg=2.013,g₁=1.955 on the degassed sample at 923K was designated toF_s⁺ centers(surface oxygen ion vacancies with a single trapped electron).When the sample was quenched from 1003K into liquid oxygenat 77K under 24 KPa O₂,[Li⁺O^-] ion pairs valued at g=2.026 andg=2.003 with superhyperfine constant a=2.0G,which resulted from ⁷Li nucleus,formed at Li⁺-substitutional site in ZnO lattice.A probable mechanism of [Li⁺O^-]ion pair formation was proposed.

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RAMAN STUDIES OF STRUCTURAL PHASE TRANSITION IN[n-C₁₁H₂₈NH₈]₂ZnCl₄

Ning GUO, Guang Fu ZENG, Shi Quan XI

中国化学快报. 1993, 4(03): 255-256.

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The perovskite type of compound [n-C₁₁H₂₃N₃]₂ZnCl₄(abr.C₁₁Zn)exhibits two solid-solid phase transitions at T_c1=298.7 K and T_c2=360.1 K.A temperature dependence study of Raman spectra of C₁₁Zn provides the evidence of occurence of the structural phase transition related to the dynamics of the alkylammonium ions.The room temperature phase is ordered and contains the all-trans alkyl chains.The intermediate temperature phase presents a partial conformational disorder and liquidlike state of all conformational disorder occurs at high-temperature phase.

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A PRELIMINARY STUDY ON THE THEORY OF THE SECOND AND THIRD ORDER DERIVATIVE ADSORPTION CHRONOPOTENTIOMETRY FOR A REVERSIBLE REACTION

Hong Guang ZHANG, Wen Rui JIN, Fu Song HUANG

中国化学快报. 1993, 4(03): 257-258.

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The equations of the second and third order derivative curves of time with respect to potential for a reversible process in adsorption chronopotentiometry are derived and experimentally verified.

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TRANSMITTED ELECTRON MICROSCOPY STUDY OF ION-CONTAINING BIOMEDICAL SEGMENTED POLYETHERURETHANE FINE STRUCTURES

Hui Ying CHEN, Jing Jing SU, Yi Zhu

中国化学快报. 1993, 4(03): 259-262.

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The microphase separation extent of biomedical segmented polyetherurethanes were greatly enhanced due to the presence of sulfoalkyl pendant groups contained in the hard segments,and the hard segments were more orderly aggregated through ionic interaction.

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SURFACE PRESSURE,SURFACE POTENTIAL AND SCANNING TUNNELING MICROSCOPY STUDIES FOR N-DOCOSYLPYRIDINIUM-TCNQ MONOLAYER

Chun-Wei YUAN, Dong XIAO, Lin WANG, Zong-Han, WU Yu WEI

中国化学快报. 1993, 4(03): 263-264.

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Simultaneous measurements of surface pressure and surface potential and scanning tunneling microscopy study for N-docosylpyridinium-TCNQ monolayer were carried out.These methods allow us to get more informations on properties of the monolayer.The molecules at the final stage of compression are really in compact stack although a voluminous hydrophilic head exists in the molecule.

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MISCIBILITY AND CRYSTALLIZATION BEHAVIOR OF BIODEGRADABLE BLEND OF POLY(β—HYDROXYBUTYRATE)AND POLY(D,L—LACTIDE)—CO—POLY(ETHYLENE GLYCOL

Xian Mo DENG, Lian Lai ZHANG, Cheng Dong XIONG

中国化学快报. 1993, 4(03): 265-268.

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Studies on the miscibility of PHB/PELA blends showed that PHB and PELA were miscible in amorphous state.The crystallization behavior of PHB in the blend was strongly de-pendent on the addition of PELA component.

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MISCIBILITY AND MORPHOLOGICAL STRUCTURE OF BIODEGRADABLE BLEND OF POLY(β—HYDROXYBUTYRATE)AND POLY(D,L—LACTIDE)

Xian Mo DENG, Lian Lai ZHANG

中国化学快报. 1993, 4(03): 269-272.

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The poly(β-hydroxybutyrate)/poly(d,1-lactide)(PHB/PLA)blend was found to be immiscible,the melting point and the phase crystallinity of PHB were independent of the blend composition.Comparing with plain PHB,the blend exhibited the crystallization change and a certain improvement of the mechanical property.

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A NEW TYPE OF CHAIN COMPOUND,STRUCTURE OF TA₄(TE₂)₄TE₄I

Shui Quan DENG, Hong Hui ZHUANG, Ding Ming WU, Jin Ling BUANG

中国化学快报. 1993, 4(03): 273-274.

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Ta₄(Te₂)₄Te₄I,Mr=2381.90,Monoclinic,C2/c,a=21.987(2),b=6.153(2),c=19.936(3)Å,β=122.42(14),V=2276.7Å³,z=4,Dm=6.8(5)g/cm³,Dc=6.95g/cm³,λ(Mok_α)=0.71073Å,μ=354.0cm^-1,F(000)=3876,T=296(1)k,R=5.3%,Rw=6.8%,for 1118 unique observed reflections(1>3σ(Ⅰ)).The structure is composed of [Ta₄(Te₂)₄Te₄I]_∞ chains,which are formed by the four-nuclear butterfly cluster units "Ta₄(Te₂)₄Te₄"with the Ⅰ atoms as the bridging atoms between different cluster units.

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PREPARATION OF ULTRAFINE PARTICLE IRON-CARBONIDE CATALYST AND CHARACTERIZATION OF ITS CATALYTICAL BEHAVIOR

Jing Chang ZHANG, Ming Ming WU, Jing Yun LU, Guang Sheng GUO, Xiao Dong HE, Fu Ming YANG

中国化学快报. 1993, 4(03): 275-278.

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Studies on ultrafine particle catalyst have attracted many researchers'attention by its large surface area,higher activity and selectivity^[1-3].Based on the mechanism of α-Fe and Fe_xC_y as the catalytical active species^[4-7] this paper reports for the first time the preparation method of Fe³C ultrafine particle catalyst,from highly dispersed amorphous Fe powder and free carbon.The Fe powder and free carbon,prepared by laser pyrolysis technique,was then treated by washing and heating at high temperature protected with N₂.The catalyst prepared under different experimental conditions was characterazed by means of XRD,electronic diffraction and TEM.It shows that the crystlline grain size is in a range of 1-4nm and composed of Fe₃C and α-Fe.It has been found that the ultrafine particleironcarbonide catalyst exhibited much higher activity and selectivity to light olefins.At the standard atmosphere and 380℃ reaction temperature,the conversion of CO reached a maximum of 80%.

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INTERACTION OF COMPONENTS IN PETROLEUM CARBOXYLATE/ALKALINE/HYDROLYZED POLYACRYLAMIDE FLOODING SYSTEM

HONG DU HUANG, LIN ZHAO Jianghan

中国化学快报. 1993, 4(03): 279-280.

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The IFTs(Interfacial tension)of petroleum carboxylate/alkaline/HPAM(Hydrolyzedpolyacrylamide)flooding system with Daing crude oil and the effects of petroleum carboxylate and alkaline on viscoaity of HPAM solution were studied.There exists remarkable synergism between HPAM and petroleum carboxylate,and the introduction of HPAM into petroleum carboxylate/alkaline system leads the lowering of IFTs against Daqing crude oil,The introduction of petroleum carboxylate into solution of HPAM also leads the decreasing of viscosity,but the extent of viscosity decreasing is much lower than that caused by inorganic salts such as NaCl and CaCl₂.

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STUDIES ON POLYMERIZATION MECHANISM OF CONJUGATED DIENE WITH η³-ALLYL RARE EARTH MODEL COMPLEX

Feng Fu LI, Ying Tai JIN, Feng Kui PEI, Fo Song WANG

中国化学快报. 1993, 4(03): 281-282.

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(η^a-C₈H₅)²CeCl₅Mg₂(tmed)₂ was used as a catalyst to polymerize isoprene,Terminal ends of polyisoprene were identified as -CH₂-CH=CH,which indicates that the insertion reaction of the monomer occurred between η^a-allyl and cerium ion and gives a direct evidence for the η^a-allyl mechanism ofconjugated diene polymerzation with rare earth coordination catalysts.

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1993年, 第4卷, 第03期　刊出日期：1993-03-20

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1993年, 第4卷, 第03期 刊出日期：1993-03-20

1993年, 第4卷, 第03期　刊出日期：1993-03-20