中国化学快报

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STUDIES ON THE PRENYLFLAVONOIDS PART V.SYNTHESIS OF (±) LESPEDEZAFLAVANONE D

Fang Jie ZHANG, Hua Wu SHAO, Yu Lin LI

中国化学快报. 1993, 4(04): 283-284.

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可视化

(±)Lespedezaflavanone D,8,5'-di(γ,γ-dimethylallyl)-5,7,2',4'-tetrahydroxyflavanone,has been synthesized by the condensation of 4,6-dimethoxymethoxy-3-(γ,γ-dimethylallyl)-2-hydroxyacetophenone with 2,4-dimethoxymethoxy-5-(γ,γ-dimethylallyl) benzaldehydc followed by cyclization and demethoxymethylation.

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ETEREOSPECIFIC SYNTHESIS OF α-D-FRUCTOFURANOSIDES--SYNTHESIS OF THE OLIGO-FRUCTAN DIASTEREOISOMERS

Biao YU, Yong Zheng HUI

中国化学快报. 1993, 4(04): 285-286.

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α-fructofuranosides were stereospecifically synthesized from 2-O-Ac-1,3,4,6-O-tetra-benzoylfructose by employing TMSOTf as a catalyst.Meanwhile,one diastereoisomer derivative of sucrose and two of fructan oligomers were synthesized.The structure of all products were confirmed by ¹³C-NMR and ¹H-NMR spectra.

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A DIACETYLENE CONTAINING α-NITRONYL NITROXIDE--SYNTHESIS,CRYSTAL STRUCTURE AND MAGNETIC CHARACTERIZATION

De Qing ZHANG, Wen Sheng ZhOU, Dao Ben ZHU

中国化学快报. 1993, 4(04): 287-288.

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The mono-α-nitronyl nitroxide substituted diacetylene was synthesized and its structure was established by EA,FAB-MS,IR,ESR and x-ray diffraction analysis.Using the Extracting Sample Magnetometer,its magnetic properties was investigated,and the results indicate that this compound possesses antiferromagnetic properties.

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FACILE SYNTHESIS OF 4-AMINO-4-DEOXY-4'-DEMETHYLEPIPODOPHYLLOTOXIN

Zhi Guang WANG, Wei Yong MA, Chun Nian ZHANG

中国化学快报. 1993, 4(04): 289-290.

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4-Amino-4-deoxy-4'-demethylepipodophyllotoxin has been directly synthesized from 4'-demethylepipodophyllotoxin and HN₃ in the presence of BF3·Et₂O,followed by hydrogenation with palladium on charcoal as catalyst.

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STUDY ON THE SYNTHESIS OF TETRACYCLIC DITERPENOID 7 Preparation of the Key Intermediate 5 for the Synthesis of Grandiflorenic Acid and its Analogues

Yun Xing CHENG, Wei Shan ZHOU

中国化学快报. 1993, 4(04): 291-294.

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The key intermediate 5 for synthesis of the contragestationally active diterpenoid grandiflorenic acid (1) and its analogues 2 and 3 was prepared and an acetyl transposition reaction occurred in the SeO² oxidation of 8.

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SYNTHESIS OF 3-BUTYLIDENE-5-HYDROXYPHTHALIDE

Shao Bai LI, Zhi Wei WANG, Xiao Ping FANG, Yu Lin LI

中国化学快报. 1993, 4(04): 295-296.

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3-Butylidene-5-hydroxyphthalide(1) was prepared from 4-hydroxybenzoic acid (2).

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TOTAL SYNTHESIS OF SQUAMOSAMIDE

Xiao Shen JI, Xiao Tian LIANG

中国化学快报. 1993, 4(04): 297-298.

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The first synthesis of squarnosamide,a new compound isolated from Annona squamosa,was achieved in seven steps.The over all yield was 14%.The compound was identified by ¹H,¹³CNMR and MS.

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STUDIES ON THE DEMETHYLATION-ALKYLATION REACTION OF ACETOPHENONES VIA 2-(1,3-DITHIAN-2-YLIDENE)-1-ARYLETHENONES

Qun LIU, Bai Ling XU, Hong Wu ZHAO

中国化学快报. 1993, 4(04): 299-302.

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2-(1,3-dithian-2-ylidene)-1-arylethenones 3 Via chemoselective 1,2-addition with methyl,ethyl,phenyl,allyl,and benzyl Grignard reagents afforded the corresponding alcohols (4).Catalyzing by silica gel,the alcohols 4 were converted to the aryl.ketones (5).The entire process represent a demethylation-alkylation reaction of acetophenones.The mechanism of reaction are proposed and the structure requirement for the conversion of the alcohols (4) was discussed.

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A NOVEL COUPLING REAGENT (PENTAFLUOROPHENYL DIPHENYLPHOSPHPATE) FOR THE PEPTIDE SYNTHESIS

Shao Qing CHEN, Jie Chang XU

中国化学快报. 1993, 4(04): 303-306.

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Pentafluorophenyl diphenylphosphate was found to be a novel convenient coupling reagent for the peptide synthesis with several advantages.Higher yield and lower racemization were found with this reagent than DCCI.

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PERFLUOROOCTANESULFONIC ACID CATALYZED FRIEDEL-CRAFTS ALKYLATION WITH OLEFINS IN GAS-LIQUID PHASE

Xiang Kai FU, Wan Li PU, Bi Kuei LUO, Chuan Yue DENG

中国化学快报. 1993, 4(04): 307-310.

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Solid superacid perfluorooctanesulfonic acid (POSA) catalyzed Friedel-Crafts alkylation of aromatic hydrocarbons with olefins in gas-liquid phase.The alkylations gave good yields with simple operation and easy work up.The amount of the catalyst used in the reactions was small and could be reused.The optimum temperature of the reactions and the effect of the amount of the catalyst used in the reactions are also discussed.

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SYNTHESIS AND CHARACTERIZATION OF NEW LIQUID CRYSTALLINE POLYURETHANE

De Li WANG, Xiao Zu HAN, Da Wei CAI, Lian Ying XIAO, Xiao Fu XUE, Zhi Shen MO

中国化学快报. 1993, 4(04): 311-312.

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A new Schiff base diol,4,4'-[3-methoxy-4-(2-hydroxy)-ethoxy] azomethine biphenyl (MHAMB),was synthesized,which was copolynerized with PEC-600 and TDI to obtain a blook polyurethane.The monomer and the polymer were charaoterized by eaploying IR,NMR and elemental analysis,Liquid crystallline phase transitions were studied by polarized aiorograph.

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REACTION OF ORGAINIC-TELLURONIUM YLIDE XI.A FACILE SYNTHESIS OF DERIVATIVES OF BISCYCLOPROPANE

Jiang Guo SHAO, Jing Feng ZHOU, Chang Qing LIU, Qi ZHONG

中国化学快报. 1993, 4(04): 313-314.

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可视化

Some telluronium salts react easily with 1,4-bis(3-substituted phenyl-3-oxo-1-propenyl) benzene and 1,5-disubstituted phenyl-1,4-pentadien-3-one to afford derivatives of biscyclopropanes in 61.8-88.8% yield.

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TELLURIUM-CATALYZED DEPROTECTI ON OF ARYL CHLOROACTATES BY SODIUM BOROHYDRIDE

Xian HUANG, Li Ming JIANG

中国化学快报. 1993, 4(04): 315-316.

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可视化

In the presence of catalytic amounts of tellurium,aryl chloroacetates can be cleaved by sodium borohydride and regenerate parent phenols in good yields.

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PALLADIUM-CATALYZED ARYLATION OF α-CYANOSULFONES UNDER PHASE TRANSFER CONDITIONS

Xian HUANG, Shan Hui JIANG

中国化学快报. 1993, 4(04): 317-318.

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α-Aryl-α-cyanosulfones are prepared under mild conditions with good yields by using palladium-catalyzed coupling reaction between aryl halides and α-cyanosulfones in the presence of phase transfer catalyst.

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HYDROXYLATION OF BENZENE BY HETEROPOLY ACIDS (SALTS) CONTAINING VANADIUM

Ru Dan HUANG, Xin Hong LU, Bao Jian ZHANG, En Bo WANG, Jin Chang LI, Jing SHI

中国化学快报. 1993, 4(04): 319-320.

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Direct hydroxylation of benzene catalyzed by vanadium-containing heteropoly compounds with Keggin or Dawson structure has been investigated.The effects of several factors upon the hydroxylation reaction have also been examined.It is indicated that the highest yield of phenol reached 76% (based on H,O,) with 99.4~100% selectivity.

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TWO NEW STEROIDAL ALKALOIDS,DONGBEININE AND DONGBEIRINE,FROM FRITILLARIA THUNBERGII MIO.VAR.CHEKIANGENSIS

Jian Xing ZHANG, Ai Na LAO, Ren Sheng XU

中国化学快报. 1993, 4(04): 321-322.

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Two new D/E trans-5d-cevanine alkaloids,Dongbernine and Dongbeirine,have been isolated from Fritillaria thunbergii Miq.var.chekiangensis together with six known compounds,peimine,peiminine,isoverticine,verticindiol,B-sitosterol daucoterol.

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NEW SESQUITERPENES FROM LIGULARIA VEITCHIANA

Yu ZHAO, Zhong Jian JIA

中国化学快报. 1993, 4(04): 323-326.

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Two new eremophilane derivatives and one new nor-sesquiterpene were isolated from Ligularia veitchiana.Their structures were elucidated by spectroscopic methods and 2D-NMR techniques and shown to be 1β,10β-epoxy-6β-(2'-semialdehyde acetal hydroxymethylacryloyloxy)-8β-ethoxy-eremophil-7(11)-en-12,8α-olide(1),1β-hydroxy-Δ⁶,Δ⁹-8-oxo-eremophil-(12)-oic-acid (2) and 1β-hydroxy-Δ⁶,Δ⁹-8-oxo-11-nor-11-hydroxyeremophiladiene(3).

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A CIDNP STUDY OF THE PHOTOREACTIONS OF METHYLFURANS WITH CHLORANIL

Ling jiang CHENG, Han Cheng YUAN, Er Cheng LI, Bao Zhen YAN, Jian Hua XU, Guang Zhi XU

中国化学快报. 1993, 4(04): 327-330.

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The CIDNP observations indicated that photoreaction of methylfurans with chloranil resulted not only furylmethyl hydroxyphenyl ethers via radical pairs but induced furyl radical isomerization to the derivatives of cyclopropene,propadiene and pyran.

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PHOTO-CIDNP STUDIES OF PHTHALIMIDE DERIVATIVES IN THE PRESENCE OF TRIETHYLAMINE

Ling Jiang CHENG, Han Cheng YUAN, Hua Pin PU, Bao Zhen YAN, Er Cheng LI, Jian Hua XU, Jin Shi MA, Guang Zhi XU

中国化学快报. 1993, 4(04): 331-334.

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可视化

The photoreactivity of some phthalimides was tested by CIDNP studies on the reactions with triethylamine.

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THE KINETIC STUDIES ON THE PHOTOISOMERIZATION OF 1,2-DISUBSTITUTED ETHYLENES

Ling Jiang CHENG, Qing Qi CHEN, Han Cheng YUAN, Jin Shi MA, Bao Zhen YAN, Guang Zhi XU

中国化学快报. 1993, 4(04): 335-338.

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An NMR study on the kinetics of photoisomerization of some important 1,2-disubstituted ethylenes are presented in this study.

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PHOTOINDUCED INTRAMOLECULAR ELECTRON TRANSFER IN A NOVEL ZINC PHTHALOCYANINE-VIOLOGEN-FERROCENE TRIAD SYSTEM

Ji Xiang LIU, Qing Fu ZHOU, Hui Jun XU

中国化学快报. 1993, 4(04): 339-342.

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A novel triad system zinc phthalocyanine-viologen-ferrocene has been synthesized.Photoinduced intramolecular electron transfer in the new triad system was investigated by fluorescence quenching experiment and nanosecond flash photolysis technique,giving a final long-living chargeseparated state.A mechanism of two-step charge separation was suggested.

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CAPILLARY ZONE ELECTROPHORESIS OF NONOSACCHARIDES

Rui Feng YAO, Yi CHEN, Li Wen CHANG

中国化学快报. 1993, 4(04): 343-346.

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A method for the analysis of monosaccharides derived from glycoproteins and glycolipids was described using the newly developed technique of capillary zone electrophoresis (CZE).It is found that,at ca.0.5-5 nL injection,CZE can offer a high resolution of most monoses from glycoprotein and glycolipids.A mixture of amino-and non-aminomonosaccharides,which is difficult to separate with chromatographic methods,was separated completely by CZE in borate buffer after the monosaccharides were derivatized with 1-naphthylamine.

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EASTMAN-AQ/Ni(Ⅱ) MODIFIED ELECTRODE DETECTION OF CARBOHYDRATES AND AMINO ACIDS

An Hua LIU, Er Kang WANG

中国化学快报. 1993, 4(04): 347-350.

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An Eastman-AQ/Ni(Ⅱ) chemically modified electrode (CME) produced by "double coating steps" deposition of Eastman-AQ/Ni(Ⅱ) film and Ni(Ⅱ)-coating crystalline species onto glassy carbon instead of metallic nickel electrode exhibited stable electrocatalytic oxidation of numerous α-hydrogen compounds including carbohydrates,amines and amino acids.Determination of glucose in FIA on the CME,the linear response concentration range was bstween 1.0×10^-5 and 5.0×10^-2 mol/L and the detection limit was 5.0×10^-6mol/L.The stability of the CME was adequate for routine quantitative application.

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IDENTIFICATION OF DOUBLE BOND POSITION IN HEXADECENYL ACETATES BY MASS SPECTROMETRY

Gu YUAN, Michio HORIIKE, Chisato HIRANO

中国化学快报. 1993, 4(04): 351-352.

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A method for locating double bond in hexadecenyl acetates has been developed by analyzing the mass spectral patterns on a fuzzy classification.The procedure was tested with the spectra of Δ^2- to Δ¹⁵-isomers and the original double-bond position in these acetates was located unambiguously.

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HOMOGENEOUS ENZYME IMMUNOASSAY OF SERUM AFP BY FLUORIMETRIC KINETIC METHOD

Qing Ge LI, Yi Bing ZHAO, Jin Gou XU, Xian Zhi HUANG, Guo Zhen CHEN

中国化学快报. 1993, 4(04): 353-354.

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The activity of the Ab-bound enzyme (HRP) changed after immunochemical reaction,and can be indicated by a sensitive fluorimetric kinetic method.The finding set the stage for developing sensitive homogeneous immunoassay.AFP was measured as an example.

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IN-SITU DISTANCE RESOLVED OPTICALLY TRANSPARENT THIN-LAYER MICROSCOPIC FTIR SPECTROELECTROCEMISTRY. ESTIMATION OF THE ELECTROCHEMICAL CONCENTRATION-DISTANCE PROFILE

Xiang Qin LIN, Zhi Li LI

中国化学快报. 1993, 4(04): 355-358.

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An in-situ optically transparent thin-layer microscopic FTIR spectroelectrochemical cell was constructed.Using this cell,we characterize a concentrationdistance profile in the electrochemical diffusion thin-layer by in-situ adjusting the focal point at different distances to the electrode surface.

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STUDIES ON VOLTAMMETRIC BEHAVIOUR OF 2-ANTIEPILEPSIRINE

Qi Long LI, Cui Ling MA, Xin Yu LIU, Jun SHANG

中国化学快报. 1993, 4(04): 359-360.

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In a supporting electrolyte containing 0.6mol/L H₂SO₄,a sensitivity derivative wave of 2-AES is formed by oscillopolarography.The peak potential is-1.01V (vs.SCE),The change of peak height with the concentration of 2-AES is linear in the range from 3.0×10^-7 to 8.0×10^-6mol/L.The detection limit is 1.0×10^-7mol/L.The electrode reaction mechanism is discussed.

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APPLICATION OF SURFACE-ENHANCED RAMAN SPECTORSCOPY FOR CHARACTERIZING HUMIC SUBSTANCES

Tong Wen NI, Yu Hui YANG

中国化学快报. 1993, 4(04): 361-362.

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Surface-enhanced Raman Spectroscopy (SERS) has been used to characterize hurnic substances.By using HNO₃-roughened silver foils as the enhancing surface,both fluorescence quenching and strong SERS signals have been observed at the same time.The results obtained herein show that SERS is a particularly sensitive and highly selective technique for the characterization of humic substances in the environment.#br#Humic substances axe receiving ever-inereasing attention because of their importance in the environment.Very recently,we have reported the first successful application of Raman spectroscopy for characterizing humic substances.In this present paper,the application of surface-enhanced Raman spectroscopy (SERS) for humic substances has further been investigated.To our knowledge,no such studies have previously beenreported.The results obtained herein dearly demonstrate that SERS has a great deal of promise as ananalytical method for "In Situ" characterizing humic substances in the environment.

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STUDIES ON THE ASYMMETRIC DECOMPOSITION OF D,L-LEUCINE INDUCED BY ⁶⁰Co γ-IRRADIATION

Wen Qing WANG, Jian JIANG, Yu Rong ZHOU, Ji Lan WU

中国化学快报. 1993, 4(04): 363-365.

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Sublimed D-,L-,and DL-leucine under vacuum were subjected to ⁶⁰Co γ-irradiation with different doses.The enantiomeric compositions of samples were determined by chirasilval capillary column gas chromatography,and the relative yields of radiolytic products (H₂,CO₂ and NH₃) were measured by packed column gas chromatography.The obtained data showed the peak area ratios D/L of DL-leucine after different absorbed doses of irradiation are all the same as that of samples with no irradiation,within the limit of error.So are the ratios for the separately irradiated D-and L-leuicne.This suggests that no asymmetric decomposition was found.The relative yields D/L of radiolytic products (H₂,CO₂ and NH₃) arevery close to 1.00,indicating that the D-leucine cleavage rate was the same with that of the L-leucine.From the view of dissipative structure,an explanation for the result was presented.

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SYNTHFESIS,STRUCTURE AND RFACTION OF TETRAMETHYL-DISILANDIYL DICYCLOPENTADIENYL TETRACARBONYL DI-IRON

Xiu Zhong ZHOU, Huai Lin SUN, Chui Hua KONG, Ru Ji WANG, Hong Gen WANG

中国化学快报. 1993, 4(04): 367-368.

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The title compounds (Me₂SiSiMe₂) (η-RC₅H₃)Fe(CO)(μ-CO) ₂(R:H(1a),Me(1b)) were prepared by heating a solution of RC₅H₄ (Me₂SiSiMe₂) C₅H₄R and Fe(CO)₅ in xylene atreflux. (1a) and (1b) can convert into their isomers Me₂Si (η-RC₃H₃) Fe(CO)₂ ₂(R:H(2a),Me(2b)) under the reaction conditions.The crystal and molecular structures of (1a), (2a) and (2b) were determined by X-ray diffraction.

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OXIDATION OF Tb(Ⅲ)IN THE HETEROPOLY-TUNGSTOPHOSPHATE COMPLEX

Wan Sheng YOU, Yuan Peng GU

中国化学快报. 1993, 4(04): 369-370.

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It has first been reported that Tb (Ⅲ) is oxidated by K₂S₂O₈ in the heteropolytungstophosphate complex.The complex ion, [Tb(Ⅳ)(PW₁₁O₃₉)₂]^10-, is stable in aqueous solutiononly for hours,being graduately reduced to[Tb(Ⅲ)(PW₁₁O₃₉)2]^11-.It is red-brown,with absorption band at about 420 nm.

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PHOTOSPLITTING OF WATEM AT THIN FILM IRON OXIDE ELECTRODES

Zheng Yu Zhou, Li Fu JIANG, Jian Zhou ZHANG

中国化学快报. 1993, 4(04): 371-372.

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both theoretical and experimental findings of the photoresponse for water spliting of the pyrolytically prepared thin film iron oxide electrodes are given.Further,the spray time and the corresponding thickness of the Fe₂O₃ thin film were optimized to have maximum photoresponse.The effect of iodine doping on photoresponse of iron oxide was investigated.

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PREPARATION,IDENTIFICATION AND INTERFACIAL ACTIVITIES OF PETROLEUM CARBOXYLATE AS SURFACTANT FOR CHEMICAL FLOODING

Hong De HUANG, You Zhen YANG, Ji Xin TANG, Cheng Quan HE, Rong Ming ZHANG, Song Mei ZHANG

中国化学快报. 1993, 4(04): 373-376.

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可视化

Petroleum carboxylate that may be suitable for tertiary oil recovery have been produced inexpensively from the fractions of Daqing crude oil by a two step process.The feed stock was first oxidized in the vapor phase,followed by reaction of the oxidized products with sodium hydroxide.Dilute solutions of sodium carboxylates were produced and show ultralow (10^-2mN/m) interfacial tensions (IFTs) against a variety of hydrocarbons with a wide range of ACN (Alkane Carbon Number).Infrared spectroscopy was used to identify the functional groups in the oxidized and the saponified products.

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1993年, 第4卷, 第04期　刊出日期：1993-04-20

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1993年, 第4卷, 第04期 刊出日期：1993-04-20

1993年, 第4卷, 第04期　刊出日期：1993-04-20