2000 Volume 11 Issue 1

A Stereoselective Approach to S-Vinyl Thioesters from Alkynes, Elemental Sulfur and Acyl Chlorides
Jun Hua WANG , Qing XU , Xian HUANG
2000, 11(1): 1-2
[Abstract](427) [FullText HTML] [PDF 69KB](2)
Abstract:
A facile, stereoselective synthesis of S-vinyl thioesters from easily available starting compounds and reagents is showed.
Intramolecular Aldol Condensation of α-Oxo Ketene Dibenzylthioacetals:A Facile Route to Substituted Thiophenes
Mang WANG , Qun LIU , Mei Xing ZHAO , Li Min WANG
2000, 11(1): 3-4
[Abstract](527) [FullText HTML] [PDF 62KB](2)
Abstract:
A new method for the synthesis of substituted thiophenes was through intramolecular aldol condensation of α-oxo ketene dibenzylthioacetals. All products were confirmed with IR, 1H NMR and elemental analysis.
Addition of Organosamarium Reagents to α, β-Unsaturated Esters
Yun Fa ZHENG , Wei Liang BAO , Yong Min ZHANG
2000, 11(1): 5-8
[Abstract](463) [FullText HTML] [PDF 115KB](3)
Abstract:
Allylsamarium bromide reacts with α, β-unsaturated esters and α-alkyloxy carbonyl α, β-unsaturated esters to give 1, 2-addition and 1, 4-addition products respectively.
Synthesis of a New Chiral Cyclic β-Amino Alcohol
Zong Xuan SHEN , Jing LIANG , Ya Wen ZHANG
2000, 11(1): 9-10
[Abstract](448) [FullText HTML] [PDF 64KB](0)
Abstract:
A new chiral cyclic β-amino alcohol (R)-1-(1'-amino-2'-naphthylethyl)-cyclopentanol 2, which had not been reported previously, was prepared from (R)-3-(2-naphthyl)-alanine 3.
The Synthesis of 4-Arylcarbonyl-3-methoxycarbonyl-2-phenylfurans by Friedel-Crafts Acylation Reactions
Shrong Shi LIN , Jun Hua YU , Jian Mei WANG , Bo YANG , Xiu Lin YE
2000, 11(1): 11-14
[Abstract](475) [FullText HTML] [PDF 162KB](0)
Abstract:
Keto esters 8, 4-arylcarbonyl-3-methoxycarbonyl-2-phenylfurans, potential precursors of the synthesis of furofuran lignans, were obtained from dimethyl 2-phenylfuran-3, 4-dicarboxylate 2. Diester 2 was selectively hydrolyzed to monoacid 6 followed by converting to its acid chloride 7. Friedel-Crafts acylation reactions of 7 with aromatic compounds afforded keto esters 8. The geometric structures of 8 and its precursors were elucidated and verified by NMR spectra.
Total Synthesis of Machilin A
Wen Xin GU , An Xin WU , Qiang GAO , Xin Fu PAN
2000, 11(1): 15-16
[Abstract](452) [FullText HTML] [PDF 62KB](0)
Abstract:
Machilin A, isolated from the bark and root of Machilus thunbergii Sieb. et Zucc. , was synthesized in eight steps from piperonal, with the coupling reaction as a key step.
Studies on the Synthesis and Property of A New Podand-armed Calix[4]arene Derivative
Yan Jun XING , Zhi Xian ZHOU , Li MA , Zhen Wei LU
2000, 11(1): 17-18
[Abstract](466) [FullText HTML] [PDF 71KB](1)
Abstract:
A new ligand 25, 26, 27, 28-tetrakis[2-(o-methoxyphenoxy)ethoxy]calix[4]arene 3 was synthesized by direct base-strength-driven O-alkylation of calix[4]arene 1. 3 has been used as ionophore for cesium selective PVC membrane electrode. The extraction for cesium and sodium with 3 have been also studied.
Synthesis and Herbicidal Activities of N'-(substituted pyrimidin-2-yl)-N-Substituted Phenoxyacetyl Thiourea Derivatives
Si Jia XUE , Jin Shan ZOU , Hai Jian YANG
2000, 11(1): 19-20
[Abstract](456) [FullText HTML] [PDF 76KB](0)
Abstract:
Fifteen N'-(substituted pyrimidin-2-yl)-N-substituted phenoxyacetyl thioureas were synthesized and tested for biological activities. All of them are new compounds and their structures were confirmed by IR. 1HNMR. MS and elemental analysis. Some of the target compounds showed excellent inhibitory activities against root and stalk of dicotyledon plant (such as radish), and selective on monoctyledon plant (such as rice).
Synthesis and optical limiting in copolymers of C60 and 1-phenyl-1-butyne
Hong Yao XU , Shan Yi GUANG , Ben Zhong TANG
2000, 11(1): 21-22
[Abstract](449) [FullText HTML] [PDF 112KB](0)
Abstract:
While WCl6-Ph4Sn is a poor catalyst for the polymerization of 1-phenyl-butyne (PB) at room temperature, it effectively polymerizes PB in the presence of C60, giving high molecular weight polymers in high yields. The polymer is soluble in THF and chloroform and spectroscopic analysis reveals that C60 has copolymerized with PB. Thus, C60 plays dual roles of comonomer and cocatalyst in the acetylene polymerization. The copolymers strongly attenuate 532-nm laser pulses, whose limiting performance is superior to that of parent C60.
Metal 2-Hydroxy-1-Naphthaldehyde Thiosemicarbazone (Me-HNT) Complexes-A New Kind of Biomimic Enzyme Catalyst
Ming DU , Fang Zhen LIANG , Bo TANG , Yun Jing LUO , Han Xi SHEN , Bin TENG , Yan LIU
2000, 11(1): 23-26
[Abstract](511) [FullText HTML] [PDF 168KB](2)
Abstract:
Metal (Me=Fe(Ⅲ), Mo(Ⅵ), Mn(Ⅱ), Co(Ⅱ), Ni(Ⅱ), Zn(Ⅱ) and Cu(Ⅱ)) 2-hydroxy-1-naphthaldehyde thiosemicarbazone complexes (MeHNT) were synthesized and used as mimic-enzyme catalysts to mimic the active group of horseradish peroxidase (HRP). The results showed that Fe-HNT, Mo-HNT are effective catalysts, which have similar catalytic activity as HRP. The sequence of catalytic activities of tested biomimic peroxidas is Mo-HNT> Fe-HNT> Zn-HNT> Ni-HNT> Mn-HNT. Among them, Fe-HNT is used as a mimic-enzyme catalyst in determination of ascorbic acid and glucose by coupling the catalytic reaction of glucose oxidase.
Synthesis of Polymer-Bonded Quaternary Ammonium Type Metal Porphyrins
Zao Ying LI , Cong LI , Xu Ye WU
2000, 11(1): 27-28
[Abstract](453) [FullText HTML] [PDF 97KB](0)
Abstract:
The reaction of pyrrole with 4-hydroxybenzaldehyde and 4-pyridinecarboxaldehyde afforded new porphyrin ligand 1. Treatment of 1 with copper(Ⅱ) acetate, cobalt (Ⅱ) acetate gave complexes 2-3 respectively. 2 and 3 reacted with Merrifield's peptide resin produced 4 and 5. Complexes 4 and 5 reacted with methyl iodide respectively gave 6-7. The new compounds 1-7 have been identified by 1H NMR, IR, MS and UV-visible spectra, elemental analysis and AES.
Facile Synthesis of Chiral Conjugated Polymer Based on BINOL Skeleton
Chun E DONG , Yong Gang ZHI , Zuo Long YU , Liang Fu ZHANG , Albert. S. C. CHAN
2000, 11(1): 29-30
[Abstract](485) [FullText HTML] [PDF 88KB](0)
Abstract:
A new type of chiral conjugated polymers 6a-d has been synthesized by the reaction of (R)-2, 2'-dihydroxy-1, 1'-binaphthyl-6, 6'-dicarbaldehyde 5 with corresponding diamine in the presence of acetic acid.
A Proposed Mechanism of Photocatalytic Oxidation of Trichloroethylene in Gas Phase
Gong Hu LI , Hu Lan MA , Wei Zhu AN
2000, 11(1): 31-34
[Abstract](465) [FullText HTML] [PDF 198KB](0)
Abstract:
GC/MS has been used to identify gas phase products and intermediates formed during the gas phase photocatalytic oxidation of trichloroethylene (TCE) on TiO2 with low BET surface area. A new byproduct, oxalyl choloride (ClCOCOCl) was detected together with other byproducts such as COCl2, CHCl3, DCAC and C2HCl5. Firstly the method of perturbation on the reaction system was conducted. Very little amount of water was carried into the feed gas and subsequent changes were observed. The discussion based on the product distribution changes led to a postulated mechanism consisting of two stages.
Mechanism of cleaving DNA through hydrolysis of a novel complex of Mg containing dien ligand
Pin YANG , Ai Xin SONG , Xiao Yi FAN
2000, 11(1): 35-36
[Abstract](456) [FullText HTML] [PDF 105KB](0)
Abstract:
A series of metal complexes were designed and synthesized and a novel binuclear magnesium complex has been selected, namely[Mg2(dien)Cl(OH2)2]Cl2·H2O (dien=diethylene-triamine), which can cleave the plasmid pBR322 DNA effectively in close to physiological condition without adding any external materials. Through biological and chemical methods, especially the comparative experiments, we find the interaction between the complex and DNA belongs to hydrolytic mechanism.
Cypripediquinone A, a new phenanthraquinone from Cypripedium macranthum (Orchidaceae)
Jian Hua JU , Jun Shan YANG , Jin LI , Pei Gen XIAO
2000, 11(1): 37-38
[Abstract](469) [FullText HTML] [PDF 96KB](0)
Abstract:
A new phenanthraquinone, cypripediquinone A, was isolated from the rhizome of Cypripedium macranthum (Orchidaceae) and its structure was established as 2, 4, 7-trimethoxy-9, 10-phenanthraquinone mainly by spectroscopic analysis.
A Cytotoxic Saponin with Two Monoterpenoids from Albizia julibrissin
Kun ZOU , Jing Rong CUI , Yu Ying ZHAO , Ru Yi ZHANG , Jun Hua ZHENG
2000, 11(1): 39-42
[Abstract](462) [FullText HTML] [PDF 132KB](1)
Abstract:
A new cytotoxic saponin (1), Julibrosides J27, was isolated from the stem barks of Alibizia. julibrissin by chromatography, and the structure was elucidated as 3-O-β-D-xylopyranosyl-(1→2)-β-D-fucopyranosyl-(1→6)-β-D-glucopyranosyl-21-O-[(6S)-2-trans-2-hydroxymethyl-6-methyl-6-O-[4-O-((6S)-2-trans-2-hydroxylmethy 6-methyl-6-hydroxy)-2, 7-octadienoyl-β-D-quinovopy-ranosyl]-2, 7-octadienoyl}-acacic acid-28-O-β-D-glucopranosyl-(1→3)-[(α-L-arabinofuranosyl-(1→4)]-α-L-rhamnopyranosyl-(1→2)-β-D-glucopyrnosyl ester based on spectral and chemical evidences.
Two New Diterpenoids from Isodon rubescens
Bao Lin LI , Shao Nong CHEN , Zhi Xian SHI , Xuan TIAN , Yao Zu CHEN
2000, 11(1): 43-44
[Abstract](506) [FullText HTML] [PDF 87KB](3)
Abstract:
Two new diterpenoids taibairubescensin A (1) and B (2) have been isolated from Isodon rubescens. The structures of compound 1 and 2 were elucidated as 2β, 3β-diacetoxy-11β, 13α-dihydroxy-ent-kaur-16-en-15-one (1) and 3β, 11β-diacetoxy-2β, 6α-dihydroxy-ent-kaur-16-en-15-one (2) on the basis of spectroscopic analysis.
Triterpenoids from Fuscoporia obliqua
Jian HE , Xiao Zhang FENG , Bin ZHAO , Yang LU
2000, 11(1): 45-48
[Abstract](485) [FullText HTML] [PDF 131KB](1)
Abstract:
Two new lanosta triterpenoids, 3β, 22α-dihydroxy-lanosta-8, 24E-diene-25-peroxide, 3, 22α, 25-trihydroxy lanosta-8, 24E-diene were isolated from the petroleum ether extracts of Fuscoporia obliqua and their structures had been determined by spectral data, chemical method and X-ray crystallographic analysis.
A New Triterpenoid Saponin from the Seeds of Vaccaria segetalis
Sheng Min SANG , Min Liang ZOU , Ai Na LAO , Zhong Liang CHEN , Jun UZAWA , Yasuo FUJIMOTO
2000, 11(1): 49-52
[Abstract](441) [FullText HTML] [PDF 117KB](0)
Abstract:
A new triterpenoid saponin, named segetoside k, has been isolated from the seeds of Vaccaria segetalis. On the basis of chemical reaction and spectral analysis, the structure of segetoside K was established as:olean-12-ene-23α, 28b-dioic acid 3b, 16a-dihydroxy-28-O-[β-D-glucopyranosyl-(1→3)]-β-D-glucopyra-nosyl-(1→2)-β-D-glucopyranosyl-(1→6)-β-D-gluco-pyranoside(1).
Two New Gallotannins from Pistacia weinmannifolia
Ai Jun HOU , Li Yan PENG , Yan Ze LIU , Zhong Wen LIN , Han Dong SUN
2000, 11(1): 53-56
[Abstract](442) [FullText HTML] [PDF 121KB](1)
Abstract:
Two new gallotannins, pistafolins A (1) and B (2), were isolated from the leaf extract of Pistacia weinmannifolia. Their structures were determined by spectral methods.
Two New C29 Sterols from Clerodendrum colebrookianum
Hui YANG , Shuang Xi MEI , Bei JIANG , Zhong Wen LIN , Han Dong SUN
2000, 11(1): 57-60
[Abstract](467) [FullText HTML] [PDF 169KB](1)
Abstract:
From the aerial parts of Clerodendrum colebrookianum Walp. , two new C29 sterols, colebrin A and colebrin B, were isolated, along with a known compound, clerosterol. The structures of the new compounds were elucidated on the basis of spectral evidence.
Study on Chemiluminescence Reactions of Lucigenin and Reductants by Flow Injection Analysis
Zhi Jia ZHU , Jiu Ru LU
2000, 11(1): 61-64
[Abstract](462) [FullText HTML] [PDF 118KB](0)
Abstract:
The chemiluminescence reactions between lucigenin and reductants such as Mo(Ⅲ), V(Ⅱ), U(Ⅲ), W(Ⅲ), Cr(Ⅱ), Ti(Ⅲ) and Fe(Ⅱ), which were produced on-line by passing Mo(Ⅵ), V(Ⅴ), U(Ⅵ), W(Ⅵ), Cr(Ⅵ, Ⅲ), Ti(Ⅳ) and Fe(Ⅲ) through a micro Jones column, are studied in detail. Results show that the reactions can be used directly for the determination of these substances. The mechanism of the reactions is also investigated.
Simultaneous Chiral Separation Using a Combinatorial Molecular Imprinting Phase
Jin Fang WANG , Liang Mo ZHOU , Xue Liang LIU , Qing Hai WANG , Dao Qian ZHU
2000, 11(1): 65-68
[Abstract](462) [FullText HTML] [PDF 142KB](0)
Abstract:
Molecular imprinting chiral stationary phase against Cbz-L-Serine (Cbz-L-Ser) and Cbz-L-Alaine (Cbz-L-Ala) were prepared utilizing acrylamide+2-vinylpyridine as combined basic functional monomers. Cross-selectivity was used to obtain simultaneous chiral separations of Cbz-DL-Ser and Cbz-DL-Ala by connecting two columns packed with Cbz-L-Ser and Cbz-L-Ala imprinted chiral stationary phase, respectively.
Synthesis and Characterization of Water-Soluble Carboxymethyl-Cyclodextrin Polymer as Capillary Electrophoresis Chiral Selector
Xue Yan SHI , Rui Fang FAN , Yue Qin ZHANG , Jun Ling GU , Ruo Nong FU
2000, 11(1): 69-70
[Abstract](467) [FullText HTML] [PDF 83KB](0)
Abstract:
The water-soluble carboxymethyl-cyclodextrin polymer (CM-CD polymer) was synthesized and used as capillary electrophoresis chiral selector. Verrapamil and thiopentorusodium were well separated using CM-CD polymer as chiral selector.
Preparation of Platinum Implanted Glassy Carbon Electrode and Electro-oxidation of Formic Acid and Formaldehyde
Cun Zhong ZHANG , Jing YANG , Xiao Lin LU , Zhong Da WU
2000, 11(1): 71-74
[Abstract](454) [FullText HTML] [PDF 138KB](0)
Abstract:
The glassy carbon substrates were bombarded with 5×1017 ions/cm2 of platinum. The surface composition of implanted electrode and concentration-depth profiles of various elements were measured by AES. The chemical state of Pt in glassy carbon electrode implanted with platinum (Pt/GC) was detected by X-ray Photoelectron Spectroscopy (XPS). The electro-oxidation of HCOOH and HCHO have been investigated on Pt/GC and smooth Pt electrodes. The results show that the platinum implanted into glassy carbon is much more active than the smooth platinum metal for electro-oxidation of HCOOH and HCHO.
The Characterization of Comblike Polymer Electrolyte by Means of NMR
Zi Jiang JIANG , Li QI
2000, 11(1): 75-78
[Abstract](461) [FullText HTML] [PDF 130KB](0)
Abstract:
The comblike polymers based on poly (styrene-co-maleic anhydride) backbone with poly (ethylene glycol) methyl ether as side chains were synthesized and characterized by 1H NMR, with the result compared with that of IR. It is found that it is both feasible and simple to synthesize this kind of compounds with the help of 1H NMR.
Direct Electrochemistry of Myoglobin in DDAB-Clay Composite Films
Nai Fei HU , Zhen LI , Hong Yan MA
2000, 11(1): 79-80
[Abstract](459) [FullText HTML] [PDF 100KB](0)
Abstract:
Ordered films were made by casting a mixture of aqueous dispersions of didodecyldimethylammonium bromide (DDAB)-clay composite and myoglobin (Mb) solution on pyrolytic graphite (PG) electrodes. The Mb-DDAB-clay film electrodes showed stable and reversible cyclic voltammetric responses in buffers and can catalyze the reduction of trichloroacetic acid (TCA).
The Electrochemical Characteristics of Multilayer Assembly of Hemoglobin and Polystyrene Sulfonate at Self-assembled Monolayer Surface
Hong SUN
2000, 11(1): 81-84
[Abstract](449) [FullText HTML] [PDF 149KB](0)
Abstract:
A multilayer film of hemoglobin (Hb) molecules and polyelectrolyte sulfonate were fabricated on a thiol self-assembled monolayers (SAMs) by electrostatic force. The Hb maintains electroactive property in the multilayer film, methylene blue (MB) incorporated into the multilayer can enhance the electron transfer rate between the Hb and the electrode surface.
Gas Phase Polymerization of Ethylene with Supported Titanium-Nickel Catalysts
Jin Min HU , Hai Hua WANG , Jiang Li WU , Qi Xing ZHANG
2000, 11(1): 85-86
[Abstract](446) [FullText HTML] [PDF 68KB](1)
Abstract:
A new ditransition-metal catalyst system TiCl4-NiCl2/MgCl2-SiO2/AlR3 was prepared. Gas phase polymerization of ethylene with the catalysts has been studied. The kinetic curves of gas phase polymerization showed a decline. The catalystic efficiency and polymerization reaction rates have a optimum value when Ni content of the catalysts was 12.5% (mol). The products obtained are branched polyethylene.
A Novel CFC-12 Hydrolysis Catalyst:WO3/SnO2
Zhen MA , Wei Ming HUA , Yi TANG , Zi GAO
2000, 11(1): 87-88
[Abstract](460) [FullText HTML] [PDF 101KB](1)
Abstract:
The catalytic hydrolysis of dichlorodifluoromethane (CFC-12) was investigated over WO3/SnO2 solid acid which was prepared by impregnating Sn(OH)4 with aqueous ammonium metatungstate followed by evaporating, drying and calcining in air. The CFC-12 conversion over WO3/SnO2 at 330℃ remained above 99.5% during 150 h on stream, however, parent metal oxides showed rare catalytic decomposition activity.
A Novel Way to Prepare γ-Al2O3 Supported SO42-/ZrO2 Solid Superacid Catalysts for n-Butane Isomerization
Ting LEI , Yi TANG , Wei Ming HUA , Jin Suo XU , Zi GAO
2000, 11(1): 89-92
[Abstract](484) [FullText HTML] [PDF 190KB](0)
Abstract:
Highly active solid superacid catalysts for n-butane isomerization, SZ/Al2O3-P, were prepared by supporting SO42-/ZrO2 (SZ) on γ-Al2O3 carrier using a precipitation method. The activities of some catalysts were enhanced significantly. The activity of the most active sample, 60%SZ/Al2O3-P, was even about 2 times more active than that of the SZ catalyst.
Synthesis and Crystal Structure of[NiL2(H2O)2](ClO4)2 L=MBPT=4-p-methylphenyl-3, 5-bis-(pyridin-2-yl)-1, 2, 4-triazole
Si Chang SHAO , Dun Ru ZHU , Tian Wei WANG , Yong ZHANG , S. Shanmuga Sundara RAJ , Hoong Kun FUN
2000, 11(1): 93-94
[Abstract](451) [FullText HTML] [PDF 98KB](0)
Abstract:
The Nickel (Ⅱ) complex, [Ni(MBPT)2(H2O)2](ClO4)2 (MBPT=4-p-methylphenyl-3, 5-bis-(pyridin-2-yl)-1, 2, 4-triazole), was synthesized and its crystal structure determined by X-ray diffraction methods. The complex adopts a distorted octahedral environment made up of two bidentate chelating MBPT ligands in the equatorial plane and two water molecules filling the axial positions.
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