2002 Volume 13 Issue 10

A Convenient Synthesis of Aromatic Fluoride by Thermal Stable Pyridinium Phase-transfer Catalyst
Ying Hong ZHU , Hui LOU , Ping LU , Jia Geng LIU , Xiao Ming ZHENG
2002, 13(10): 919-920
[Abstract](181) [FullText HTML] [PDF 646KB](1)
Using 4-Dialkylaminopyridinium salt as a thermal stable phase-transfer catalyst (PTC),the excellent results were obtained in the halogen-exchange fluorination.
Indium (III) Tribromide:An Excellent Catalyst for Biginelli Reaction
Nan Yan FU , Mei Li PANG , Yao Feng YUAN , Ji Tao WANG
2002, 13(10): 921-922
[Abstract](197) [FullText HTML] [PDF 700KB](0)
A highly efficient catalyst indium (III) tribromide is used to synthesize 5-alkoxycarbonyl-4-hydrocarbyl-3,4-dihydropyrimidin-2(1H)-ones by a three-component coupling of β-keto ester, aldehydes and urea through improved Biginelli reaction.
Novel Reaction of Nitroxide with Hantzsch Dihydropyridines
Man LU , Jian Guo FANG , Zhong Li LIU , Long Min WU
2002, 13(10): 923-925
[Abstract](212) [FullText HTML] [PDF 955KB](2)
4-oxo-2,2,6,6-tetramethylpiperidinyl-1-oxy radical (TEMPO), a nitroxide, oxidized 4-substituted Hantzsch 1,4-dihydropyridines (DHP) under UV irradiation in CH3CN to give aromatic products in good yields. A possible mechanism for the oxidation was suggested.
Synthesis of Poly(phthalazinone ether ketone) Containing Sodium Sulfonate Groups via Direct Polymerization
Shou Hai ZHANG , Xi Gao JIAN , Guo Qing WANG , Wen Xia LI
2002, 13(10): 926-928
[Abstract](202) [FullText HTML] [PDF 857KB](0)
1,2-Dihydro-4-(4-hydroxyphenyl) (2H)phthalazin-1-one (DHPZ) was sulfonated in concentrated sulfuric acid. Poly(phthalazinone ether ketone) containing pendant sodium sulfonate group was synthesized from sulfonated and pure 1,2-dihydro-4-(4-hydroxyphenyl) (2H)phthalazin-1-one, and 4,4'-difluorodiphenylketone. The sulfonated monomer and sulfonated polymer were characterized with FT-IR and 1H-NMR.
The First Total Synthesis of Isoliquiritin
Ya Ping WANG , Liang Xi LI , Qing Lian WANG , Yu Lin LI
2002, 13(10): 929-930
[Abstract](186) [FullText HTML] [PDF 667KB](0)
A first total synthesis of isoliquiritin was accomplished starting from p-hydroxybenzaldehyde and 2,4-dihydroxyacetylphenone. The key step is condensation reaction. In synthetic process need not protect the hydroxy group of reacting substance.
Enantioselective Reduction of Achiral Ketones with NaBH4/I2 Catalyzed by (S)-Ferrocenyl Amino Alcohols
Wei Yi CHEN , Jun LU , Ya Wen ZHANG , Zong Xuan SHEN
2002, 13(10): 931-932
[Abstract](173) [FullText HTML] [PDF 606KB](0)
The reduction reagents prepared from sodium borohydride, I2 and a catalytic amount of chiral ferrocenyl amino alcohols 2a-e have been successfully applied to the enantioselective reduction of ketones. The optically active secondary alcohols were obtained in moderate enantiomeric excess and high chemical yield.
Effect of Co-solvent on the Palladium Catalyzed Alkoxycarbonylation of Allyl Bromide in Supercritical CO2
Rui Qi SONG , Jian Qing ZENG , Bing ZHONG
2002, 13(10): 933-934
[Abstract](168) [FullText HTML] [PDF 722KB](0)
The effect of cosolvent on the palladium catalyst which catalyze alkoxycarbonylation of allyl bromide in supercritical CO2 has been investigated. It was found that a small amount of cosolvent such as ethanol, CH2Cl2 and cyclohexane can affect both reaction yields and selectivities largely. Ethanol was the most favorable cosolvent for increasing the total yield of unsaturated esters and the selectivity of 3-butenoic acid ester. Using cosolvent ethanol and cocatalyst FeCl2 simultaneously can lead to better reaction results.
Total Synthesis of (±)-Nimbonone and (±)-12-Ethyl-13-methoxy-8,11,13-podocarpatriene
Cheng Lu ZHANG , Ping Yan BIE , Xuan Jia PENG , Xin Fu PAN
2002, 13(10): 935-936
[Abstract](164) [FullText HTML] [PDF 717KB](1)
A facile total synthetic route to (±)-nimbonone and (±)-12-ethyl-13-methoxy-8,11,13-podocarpatriene was developed. The Wittig reaction of α-cyclocitral with (3-methoxybenzyl) triphenylphosphonium and intramolecular cyclization with BF3·Et2O in the synthetic progress were applied. In order to induce the ethyl substituent, Fiedel-Crafts acetylation and then decarbonylation had been employed.
Studies on the Total Synthesis of Hainanolide (VII)-Analysis of the Relative Stereochemistry of key Intermediate 2
Yan Wu LI , Liang HUANG
2002, 13(10): 937-938
[Abstract](163) [FullText HTML] [PDF 549KB](0)
The relative stereochemistry of an intermediate 2 in the total synthesis of hainanolide 1 was studied by various NMR spectroscopic techniques.
Diastereoselective and Enantioselective Synthesis of (1S,2S)-2-Ethyl-1-aminocyclopropane Carboxylic Acid
Yi Bo ZHOU , Jun An MA , Li Xin WANG , Qi Lin ZHOU
2002, 13(10): 939-941
[Abstract](161) [FullText HTML] [PDF 1087KB](0)
Pd(0) Complex prepared from Pd(dba)2 and chiral quinolinyl-oxazoline ligand can catalyze alkylation and cyclization reaction of 1,4-dichlorobut-2-ene 1 with anion of N-(diphenylmethylene) amino acetonitrile 2 to provide (E)-2-ethenyl-1-N-(diphenylmethylene) amino cyclopropane carbonitrile 3 with 100% de and 20% ee. Reduction of (E)-3 by diimide followed by acidic hydrolysis afforded (1S, 2S)-2-ethyl-1-aminocyclopropanecarboxylic acid 9, a natural product coronamic acid.
New Facile Synthesis of 2-Aryloxy-5-(2-furfurylidene)-4H-imidazolin-4-ones
Ming Wu DING , Jing ZHU , Su Fang SHI , Xiao Peng LIU
2002, 13(10): 942-944
[Abstract](163) [FullText HTML] [PDF 1099KB](0)
Novel 2-aryloxy-5-(2-furfurylidene)-4H-imidazolin-4-ones 6 were synthesized by aza-Wittig reaction of vinyliminophosphorane 4 with phenyl isocyanate and subsequent condensation with various substituted phenols in the presence of catalytic amount of potassium carbonate. The products are confirmed by 1H NMR, MS, IR and elementary analysis.
Synthesis and Nonlinear Optical Property of a Series of New Chromophores Containing Furan Ring as the Only Conjugation Bridge
Wei ZHANG , Jian Li HUA , Jin Gui QIN
2002, 13(10): 945-948
[Abstract](167) [FullText HTML] [PDF 1288KB](0)
This paper reports the synthesis and the nonlinear optical property of a series of new chromophores which contain furan ring as the only conjugation bridge for the first time. They are characterized by UV-VIS, FT-IR, 1H NMR, MS and elemental analysis. Their dipole moment and the first-order molecular hyperpolarizability (β) are calculated and compared with those of the analogues containing either benzene or thiophene as the conjugation bridge.
Synthesis of a New Family of Green Light Emitting Material Containing Both Hole and Electron Transporting Units
Hai Tao YU , Wan Xuan ZHANG , Wu Xin ZHOU , Teruo MASTUURA , Ji Ben MENG
2002, 13(10): 949-952
[Abstract](156) [FullText HTML] [PDF 1151KB](0)
Two new molecules containing oxadiazoles and triphenylamine-stilbene moiety were synthesized. Their luminescent properties were determined, which indicated that they had strong green fluorescent properties. All the two molecules can be used as green organic electroluminescence materials.
A New Sesquiterpene from the Alga Caloglossa Leprieurii
Xiao Hua XU , Chang Jian LIN , Jian Hua LU , Guang Min YAO , Yan Ming LI
2002, 13(10): 953-954
[Abstract](155) [FullText HTML] [PDF 655KB](0)
A new bromo-sesquiterpene 1, has been isolated from the alga Caloglossa leprieurii collected from the XiSha islands in south china sea. Its structure has been determined on the basis of spectral analysis, and The relative configuration of 1 was assigned on the basis of difference spectrum of NOE.
One New Diterpene Glucoside from the Roots of Rhododendron molle
Guan Hu BAO , Li Quan WANG , Kin Fai CHENG , Guo Wei QIN
2002, 13(10): 955-956
[Abstract](172) [FullText HTML] [PDF 710KB](0)
One new grayanane diterpene glucoside, rhodomoside A 1 was isolated from the roots of Rhododendron molle G. Don (Ericaceae). Its structure was elucidated on the basis of spectral analysis.
A New Alkaloid from Patrinia scabra
Zheng Bing GU , Gen Jin YANG , Wen Yong LIU , Ting Zhao LI , Yan QIU , Wei Dong ZHANG
2002, 13(10): 957-958
[Abstract](166) [FullText HTML] [PDF 617KB](0)
A new alkaloid has been isolated from the root of Patrinia scabra. Its structure was elucidated as 2'-acetamido-3'-phenyl propyl 2-benzamido-3-phenyl propionate by extensive spectroscopic analysis.
Two New Arylnaphthalene Lignan Glycosides from Mananthes patentiflora
Bin CHEN , Yan LIU , Chun FENG , Bo Gang LI , Guo Lin ZHANG
2002, 13(10): 959-962
[Abstract](178) [FullText HTML] [PDF 1339KB](2)
Two new diphyllin glycosides, mananthoside A (1) and B (2), together with six known compounds, were isolated from the ethanolic extract of the whole plants of Mananthes patentiflora.Their structures were determined on the basis of chemical and spectral evidences.
Two New Eremophilenolides from Ligularia sagitta
Xu Qin LI , Kun GAO , Zhong Jian JIA
2002, 13(10): 963-964
[Abstract](176) [FullText HTML] [PDF 641KB](2)
Chemical investigation of L.sagitta afforded two new eremophilenolides, which were identified as 6β-angeloyloxy-10β-hydroxy-8β-methoxy-eremophil-7(11)-en-12, 8α-olide (1) and 6β,8β-dimethoxy-10β-hydroxy-eremophil-7(11)-en-12, 8α-olide (2). Their structures were established by spectroscopic methods including 2D NMR experiments.
A New Sesquiterpene from the Roots of Lindera strychnifolia
Jian Bei LI , Yi DING , Wei Min LI
2002, 13(10): 965-967
[Abstract](186) [FullText HTML] [PDF 960KB](5)
A new sesquiterpene lactone, strychnilactone (1), together with five known sesquite-rpenoids,linderane (2), lindenenol (3), linderalactone (4), hydroxylindestenolide (5), pseudoneolinderane (6) have been isolated from the extracts of Supercritical Fluid Extraction of Lindera strychnifolia. The structure of the new compound was elucidated by means of spectroscopic analysis. And the relative configuration of 1 was assigned on the basis of NOE analysis.
Determination of the Flavonoids from Ginkgo Biloba Extract by High Performance Liquid Chromatography
2002, 13(10): 968-970
[Abstract](174) [FullText HTML] [PDF 1098KB](4)
HPLC method for analysis of the flavonoids from ginkgo biloba extract (GBE) was studied. By suitable selection of columns, symmetrical chromatographic peaks were obtained without using acidic modifier in the mobile phase, which can eliminate the time for cleaning the chromatographic system and simplify the analystic method for GBE. Experimental conditions:column:Hypersil BDS C18, 5μm×4×250 mm; column temperature:35℃; mobile phase:46% methanol-54% water; flow rate:0.7 mL/min; detection wavelength:360nm.
Electrochemical Detection of Horseradish Peroxidase at Zeptomole Level
Zhi Hui HE , Wen Rui JIN
2002, 13(10): 971-972
[Abstract](163) [FullText HTML] [PDF 539KB](0)
An electrochemical method for determination of horseradish peroxidase (HRP) was developed using a capillary catalytic system. HRP can be measured in several minutes with a detection limit of 4.8×10-12 mol/L or 47 zmol (S/N=3).
The Enantiomer Separations of Allethrone and Propargyllone Using Two Long Chain Acylated β-Cyclodextrin Derivatives as CGC Capillary Stationary Phases
Xue Yan SHI , Hong Chao GUO , Zhen QIAO , Shi Cong HOU , Min WANG
2002, 13(10): 973-976
[Abstract](160) [FullText HTML] [PDF 1130KB](0)
Using two β-cyclodextrin derivatives (CDs) with long chain of acyl groups as chiral stationary phases (CSPs) of capillary gas chromatography (CGC), the enantiomers of racemic allethrone and propargyllone were well resolved after derived with acetyl chloride. The enantiomer excess values (e.e.%) of 1S-allethrone and 1S-propargyllone were also determined successfully using these CDs.
Assay of Cysteine in Human Serum with Quinine-Ce4+ Chemiluminescence System
Li Hua NIE , Hui Min MA , Mei Hong SU , Ming SUN , Xiao Hua LI
2002, 13(10): 977-978
[Abstract](165) [FullText HTML] [PDF 847KB](0)
A sensitive and selective chemiluminescence (CL) method was developed for the determination of cysteine. This method is based on that the weak CL of cysteine oxidized with cerium (IV) can be greatly enhanced by quinine, and the total cysteine in human serum can be detected through simply diluting with water, showing a simpler analytical characteristic.
Determination of Amino Acids in Single Human Lymphocytes after On-capillary Derivatization by Capillary Zone Electrophoresis with Electrochemical Detection
Qian Feng WENG , Wen Rui JIN
2002, 13(10): 979-981
[Abstract](165) [FullText HTML] [PDF 1003KB](0)
Amino acids in individual human lymphocytes were determined by capillary zone electrophoresis with electrochemical detection after on-capillary derivatization. In order to inject cells easily, a cell injector was designed. Four amino acids (serine, alanine, taurine, and glycine) in single human lymphocytes have been identified. Quantitation has been accomplished through the use of calibration curves.
Assay of Histamine in Single Mast Cells by Capillary Zone Electrophoresis with Electrochemical Detection
Qian Feng WENG , Fang Quan XIA , Wen Rui JIN
2002, 13(10): 982-984
[Abstract](157) [FullText HTML] [PDF 952KB](0)
Capillary zone electrophoresis was employed for the analysis of histamine in single rat peritoneal mast cells using an amperometric detector. In this method, individual mast cells and then 0.02 mol/L NaOH as a lysing solution are injected into the front end of the separation capillary. A cell injector was constructed for easy injection of single cells. Histamine in single mast cells has been identified and quantified.
Carbon Fiber-gold/mercury Dual-electrode Detection for Capillary Electrophoresis
Qian Feng WENG , Wen Rui JIN
2002, 13(10): 985-987
[Abstract](168) [FullText HTML] [PDF 999KB](0)
A carbon fiber-gold/mercury dual-electrode for capillary electrophoresis is constructed.Cysteine, glutathione, ascorbic acid and uric acid can be detected simultaneously and selectively at the dual-electrode, respectively. The capillary electrophoresis/dual-electrode detection system has been used to determine these compounds in human blood samples.
Synthesis and Characterization of Small Band-gap Conjugated Polymers-Poly(pyrrolyl methines)
Wei YAN , Chain Shu HSU , Yu WEI
2002, 13(10): 988-990
[Abstract](170) [FullText HTML] [PDF 916KB](0)
A kind of small band-gap conjugated polymers-poly (pyrrolyl methines) and their precursors-(poly pyrrolyl methanes) have been synthesized by a simple method and characterized by 1HNMR, FT-IR, TGA and UV-Vis. These polymers can be dissolved in high polar solvents such as DMSO, DMF or NMP. The results reveals that the band-gap of the synthesized conjugated polymers are in the range of 0.96~1.14 eV and they all belong to the small band-gap polymers. The conductivity of doped products with iodine is in the range of semiconductor.
Hybrid Luminescent Films Obtained by Covalent Anchoring Terbium Complex to Silica-based Network
Feng Yi LIU , Lian She FU , Jun WANG , Huan Rong LI , Hong Jie ZHANG
2002, 13(10): 991-992
[Abstract](163) [FullText HTML] [PDF 660KB](0)
New monomer N-(4-carboxyphenyl)-NL-(propyltriethoxysilyl) urea (1) which acts as both a ligand for Tb3+ ion and a sol-gel precursor has been synthesized and characterized by 1H NMR, and MS. Hybrid luminescent thin films consisting of organoterbium covalently bonded to a silica-based network have been obtained in situ via a sol-gel approach. Strong line emission of Tb3+ ion was observed from the hybrid luminescent films under UV excitation.
Investigation on the Inverse Emulsion Polymerization of Acrylic Acid
Jian Fang GE , Feng Ji LU , Wen DING
2002, 13(10): 993-996
[Abstract](1119) [FullText HTML] [PDF 1020KB](18)
Polyacrylic acid particles in nano-scale were synthesized using an inverse (W/O) emulsion polymerization method. The particle size and size change of inverse micelles which solubilize a part of monomer solution was monitored by PCS (photon correlation spectroscopy) and the particles of polyacrylic acid were viewed in scanning electron microscope for the first time.It was concluded that the inverse micelles were primarily the polymerization reaction sites.
Structure and Two-photon Excited Blue Fluorescence of an Asymmetrical Substituted Stilbene
Zhi Qiang LIU , Qi FANG , Wen Tao YU , Gang XUE , Du Xia CAO , Dong WANG , Guang Ming XIA , Min Hua JIANG
2002, 13(10): 997-1000
[Abstract](161) [FullText HTML] [PDF 1371KB](0)
The single & two photon excited fluorescence property and crystal structure of a substituted stilbene-type compound trans-4-diethylamino-4'-bromostilbene (DEABS) has been reported. The results indicate that this compound has strong two photon excited blue fluorescence at 440 nm when the 700 nm laser was used as the pump source.
Study on the Interaction between Distamycin Analogs and DNA from Herring Sperm by Fluorimetry
Han LIANG , Jing Jian LI , Xiao Dong LI , Fei Li TANG , Gu YUAN
2002, 13(10): 1001-1002
[Abstract](161) [FullText HTML] [PDF 610KB](0)
The fluorescence spectra of the interaction between four new distamycin analogs and DNA from herring sperm have been studied in detail. The fluorescence quenching of the DNA by the analogs was observed, and the fluorescence intensity of the DNA was attenuated exponentially with the increasing of the analogs concentration.
Liquid Membrane Transport Behavior of Functional Substituted Crown Ethers for Amino Acids
Xin Cheng LIAO , Xing Wang WANG , Jing Chao TAO
2002, 13(10): 1003-1004
[Abstract](159) [FullText HTML] [PDF 754KB](4)
Three functional substituted crown ethers were synthesized as liquid membrane transport carriers for amino acids. The result obtained shows that this kind of ditopic ligands can transport sodium salt of amino acids in good rate value especially the one with two pyridinyl groups as binding site outside the macrocycle.
Binding Affinity of Novel Cyclodextrin Dimers to Ethyl Orange
2002, 13(10): 1005-1006
[Abstract](163) [FullText HTML] [PDF 780KB](0)
The interaction between ethyl orange (Eto, guest) and β-cyclodextrin dimers (1a~d, host) bridged with 2-t-butoxycarbonyl (Boc)-amino diacid was investigated. A remarkable synergic complexation of two cavities in host molecule was observed.
Absorption Complex between Porphyrin and Phenothiazine in Reverse Micelles
Jun Hua YU , Xue Song WANG , Bao Wen ZHANG , Yi CAO
2002, 13(10): 1007-1010
[Abstract](165) [FullText HTML] [PDF 1392KB](0)
The interaction between amphiphilic porphyrin and phenothiazine in AOT/isooctane/water reverse micelle was investigated by UV-Vis spectra. A new absorption complex between the two species is formed in such circumstances, which is ascribed to the enrichment of the components by the reverse micelle. The fluorescence quenching of CHTTP by PTH becomes more efficient after the formation of the absorption complex.
Thermoregulated Phase-separable Ru3(CO)12/PETPP Complex Catalyst for Hydrogenation of Styrene
Yan Hua WANG , Xiao Wei WU , Fang CHENG , Zi Lin JIN
2002, 13(10): 1011-1012
[Abstract](164) [FullText HTML] [PDF 667KB](0)
Thermoregulated phase-separable Ru3(CO)12/PETPP (PETPP=P[p-C6H4O (CH2CH2O)n H]3, n=6) complex catalyst was first applied in the hydrogenation of styrene. Under the conditions:P(H2)=2.0MPa, T=90℃, styrene could be completely transferred and the yield of ethylbenzene reached up to 99.5%. After simple decantation, the catalyst could be reused for ten times without decreasing in activity.
A Durable Catalyst for Vapor Phase Nitration of Benzene with Nitric Acid
Peng ZHOU , Xin Ping WANG , Tian Xi CAI
2002, 13(10): 1013-1016
[Abstract](170) [FullText HTML] [PDF 1373KB](0)
Experimental results in this work demonstrate that PW12-H2SO4/SiO2 catalyst is a good and durable catalyst for vapor phase nitration of benzene to nitrobenzene (NB) using 65% nitric acid at normal pressure. It retains the advantages of using H2SO4 as catalyst and the addition of phosphotungstic acid holds back the effusion of sulfuric acid. This new catalyst keeps high activity (the conversion of HNO3 is more than 92%), high selectivity of NB (more than 97%) and high space time yield (STY 1.5 kg NB/kg cat.h) even after 150 h on stream, under condition of 423 K, SV=3200 ml/g h.
Hydrothermal Synthesis of Pb1-1.5xLaxZr0.5Ti0.5O3 (x=0.01-0.06) Nanocrystallites
Xiu Ling JIAO , Dai Rong CHEN
2002, 13(10): 1017-1020
[Abstract](167) [FullText HTML] [PDF 1411KB](0)
Nanocrystalline Pb1-1.5xLaxZr0.5Ti0.5O3 (x=0.01-0.06, PLZT) powders with particle size from 30 to 150 nm were hydrothermally synthesized from the gels under mild conditions. The reaction conditions such as La content, reaction temperature and time were studied in detail and optimal conditions were established for synthesizing PLZT powders with different La contents.The effects of La content, alkali concentration, reaction temperature and time on the particle size were studied.
Synthesis of the Complex Fluoride LiBaF3 through a Solvothermal Process
Rui Nian HUA , Zhi Hong JIA , De Min XIE , Chun Shan SHI
2002, 13(10): 1021-1024
[Abstract](167) [FullText HTML] [PDF 1215KB](0)
The complex fluoride LiBaF3 is solvothermally synthesized at 180℃ and characterized by means of X-ray powder diffraction, scanning electron microscopy, thermogravimetric analysis and infrared spectroscopy. In the solvothermal process, the solvents, mole ratios of initial mixtures and reaction temperature play important roles in the growth of the single crystal.
MesoDyn Simulation Study on Phase Diagram of Aerosol OT/isooctane/water System
Shi Ling YUAN , Gui Ying XU , Zheng Ting CAI
2002, 13(10): 1025-1028
[Abstract](196) [FullText HTML] [PDF 1361KB](0)
A simple model, i.e. sodium di(2-ethylhexyl) sulfosuccinate (AOT) represented by one-head and two-tail beads tied together by a harmonic spring and water or isooctane by one bead,was put forward via Dissipative Particles Dynamics (DPD) simulation method. Using the changes of interfacial tension between water and oil phase, a ternary phase diagram of AOT/water/isooctane system was drawn. From the simulation, one conclusion is shown that DPD simulation can be considered as an adjunct to experiments.
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