2004 Volume 15 Issue 8

Michael Additiion of Alkyl Amine to α,β-Unsaturated Carbonyl Compounds Catalyzed by KF/Al2O3
Dan Bi TIAN , Jun ZHU , Jie Fang ZHU. Yuan Xiang SHI , JiN Tang WANG
2004, 15(8): 883-884
[Abstract](202) [FullText HTML] [PDF 683KB](0)
The β-aminocarboxylic acid derivatives were synthesized by Michael addition reaction of alkyl amine and α,β-unsaturated carbonyl compounds in the presence of potassium fluoride on alumina.
Design,Synthesis,and Hypnotic Activity of Pyrazolo[1,5-a]pyrimidine Derivatives
Song Qing WANG , Lin FANG , Xiu Jie LIU , Kang ZHAO
2004, 15(8): 885-888
[Abstract](272) [FullText HTML] [PDF 1481KB](1)
On the basis of the Zaleplon structure, novel pyrazolo[1,5-a]pyrimidines were designed and prepared for studies on their hypnotic activity.This paper reported the synthesis of twelve new 5-methyl-7-substituted-pyrazolo[1,5-a]pyrimidine-3-carbonitrile derivatives by using simple starting materials such as propane dinitrile and triethyl orthoformate.The structures of the derived target compounds were confirmed by their IR and 1H-NMR spectroscopic data.The preliminary pharmacological evaluations indicated that some compounds showed hypnotic activity, while derivative 1c was the most potent one.
A Novel Synthesis of N-Methyl-N-aryl Carbamates from Aromatic Amines and Dimethyl Carbonate Catalyzed by K2CO3/Bu4NBr
Zhen Lu SHEN , Xuan Zhen JIANG
2004, 15(8): 889-891
[Abstract](299) [FullText HTML] [PDF 1020KB](0)
A facile synthesis of N-methyl-N-aryl carbamates from aromatic amines and dimethyl carbonate (DMC) has been achieved with high yields in the presence of potassium carbonate (K2CO3) and tetrabutylammonium bromide (Bu4NBr) under solvent-free conditions.
Synthesis of Hymecromone Derivatives Containing Chiral 1,1'-Bi-2-naphthyl Moiety for Dual-mode Molecular Switch
Zi Xing SHAN , Chun Guang XIAO
2004, 15(8): 892-894
[Abstract](212) [FullText HTML] [PDF 1190KB](1)
Some hymecromone derivatives containing chiral 1,1'-bi-2-naphthyl moiety were synthesized and their photodimerizations were investigated.It was found that fluorescence intensity and optical rotation of the new chiral hymecromone derivatives could be regulated by light.This property has potential significance for developing a new type of dual-mode molecular switch.
A New Synthetic Route for Preparation of 2-Chloro-6-fluoro-benzonitrile and 2-Chloro-6-fluorobenzoic Acid
Xiao Yun LI , Qiong ZHENG , Peng YU , Chi HUANG , Jian Li DUAN , Jun Qing PENG
2004, 15(8): 895-898
[Abstract](207) [FullText HTML] [PDF 1325KB](2)
An effective synthetic route for preparation of 2-chloro-6-fluorobenzonitrile, 2-chloro-6-fluorobenzamide and 2-chloro-6-fluorobenzoic acid has been described.It includes diazotization, fluorination, ammoxidation and hydrolysis reactions.
The Effect of 19-Substituent on the Stereospecific Hydroxylation of Δ5-Steroids Using Performic Acid as Oxidant
Wei Gang LU , Jing Yu SU , Long Mei ZENG , Hong LI
2004, 15(8): 899-902
[Abstract](313) [FullText HTML] [PDF 1274KB](0)
In the studying of the stereospecific hydroxylation of different Δ5-steroids with performic acid, followed by hydrolysis with CH3OH/KOH, we found 19-substituting groups considerably affected the reaction and we put forward the mechanism.
A Novel and Efficient Catalytic System for Aerobic Oxidative Coupling of 2-Naphthol Derivatives
Li CHEN , Jing Bo LAN , Zhi Hua MAO , Xiao Qi YU , Ru Gang XIE
2004, 15(8): 903-906
[Abstract](212) [FullText HTML] [PDF 1461KB](1)
The paper reported a novel and efficient aerobic oxidative coupling reaction of 2-naphthol derivatives catalyzed by CuCu (Ⅰ or Ⅱ)N-alkylimidazole complexes in excellent yields.The crystal structure of CuCu (Ⅱ)N-methylimidazole complex to be determined by X-Ray.
Synthesis of a Photolabeling Probe for the Study of Antiviral Mechanism of Ribavirin
Qiong You WU , Xun ZHU , JIN Qiao WAN , Fan Qi QU , Ling PENG
2004, 15(8): 907-910
[Abstract](186) [FullText HTML] [PDF 1432KB](0)
Ribavirin has been used in urgency to treat SARS patients recently.In order to study its antiviral mechanism by photolabeling approach, we have synthesized and characterized 5-azido-1-(-D-ribofuranosyl-1,2,4-triazole-3-carboxiamide 1 as a photolabeling probe of ribavirin.The azidotriazole nucleoside showed rapid and clean photochemical reaction, suggesting that 1 is a promising probe to study the antiviral mechanism of ribarivin by photolabeling.
An Efficient and Mild Preparation of Vinyl Diazo Carbonyl Compounds
Wei Feng SHI , Ming MA , Jian Bo WANG
2004, 15(8): 911-914
[Abstract](168) [FullText HTML] [PDF 1246KB](0)
The combination of (CF3CO)2O/Et3N is found to be a mild and efficient dehydration condition forβ-hydroxy-α-diazo compounds.
Octopus Manganese Porphyrin with Polyglycol Chains as a Catalyst for the β-Selective Epoxidation of Cholesterol Derivatives
Run Hua LI , Yuan Cong ZHAO , Jiang WU , Jing Song YOU , Xiao Qi YU
2004, 15(8): 915-918
[Abstract](255) [FullText HTML] [PDF 1274KB](0)
Synthesis of a novel octopus porphyrin with polyglycol chains 1a was achieved.The catalytic activity of 1a's manganese complex for the epoxidation of cholesterol derivatives with PhIO give a satisfactory conversion and regioselectivity.
A New Labdane Diterpenoid from the Bark of Larix olgensis Henry var.koreana Nakai
Bao Hua YANG , Wei Dong ZHANG , Zheng Bing GU , Ting Zhao LI , Chuan ZHANG , Yun ZHOU
2004, 15(8): 919-920
[Abstract](191) [FullText HTML] [PDF 614KB](0)
A new diterpenoid was isolated from the bark of Larix olgensis Henry var.koreana Nakai.Its structure was elucidated as 5S, 9S, 10R-labda-8 (17), 13-diene-6α, 15-diol 1 by spectroscopic methods.
Neo-lignans in the Seed Crusts of Trewia nudiflora
Pei Ji ZHAO , Yue Mao SHEN
2004, 15(8): 921-924
[Abstract](247) [FullText HTML] [PDF 1382KB](1)
Four new neo-lignans were isolated from the chloroform portion of 70% ethanol extract of the seed crusts of Trewia nudiflora L., and were determined to be 9'-methoxy-7'-en-3',8:4',7-di-epoxyneolignan-3,4,9-triol 1, 9'-methoxy-7'-en-3',7:4',8-diepoxyneolignan-3,4,9-triol 2, 9'-ethoxy-7'-en-3',8:4',7-diepoxyneolignan-3,4,9-triol 3, 9'-butoxy-7'-en-3',8:4',7-diepoxy-neolignan-3,4,9-triol 4, respectively, on the basis of spectral data.The antimicrobial bioassays showed that 4 had evident inhibitory activity against Mycobacterium tuberculosis.
A New Dihydroflavone Glycoside from Glycyrrhiza uralensis
Hong Xia LIU , Wen Han LIN , Jun Shan YANG
2004, 15(8): 925-926
[Abstract](175) [FullText HTML] [PDF 756KB](0)
A new dihydroflavone glycoside was isolated from the underground parts of Glycyrrhiza uralensis.Its structure was elucidated as 7-hydroxyl-4'-O-β-D-(6"-O-α-hydroxylpropionyl) glucopyranosyl dihydroflavone by spectral methods.
MALDI-TOF Mass Spectrometry Study of the Phosphorylated Tau Peptides
Jin Tang DU , Yan Mei LI , Yu Fen ZHAO , Masatoshi NAKAGAWA , Xu Rong QIN , Tadashi NEMOTO , Hiroshi NAKANISHI
2004, 15(8): 927-930
[Abstract](193) [FullText HTML] [PDF 1454KB](0)
Fragmentation of phosphorylated Tau peptides in matrix assisted laser desorption-/ionization-time of flight-mass spectrometry (MALDI-TOF-MS) has been investigated.According to the post-source decay (PSD) in MALDI-TOF-MS, there are two different patterns of cleavage in phosphopeptides, which can be used to determine the phosphorylated site in peptides.In the synthetic tau peptides, the fragmentation at proline residue occurs strongly and this is useful to determine the structure of tau peptides.
New Phase Transfer Agent for Dye:Application for Hyperbranched Poly (ester-amine)
Teng QIU , Li Ming TANG , Xin Lin TUO , De Shan LIU
2004, 15(8): 931-934
[Abstract](179) [FullText HTML] [PDF 1063KB](0)
Hydrophilic hyperbranched poly(ester-amine) (HPEA) synthesized from diethanolamine and methyl acrylate was used as phase transfer agent for the first time to transfer methyl orange (MO) from water into chloroform.This process was quantified by UV-Vis spectra.A possible mechanism was put forward based on the formation of amphiphilic aggregates.
A New Method of Separation of Four Benzodiazepines by RP-CEC
Jin Lan ZHANG , Tong Hui ZHOU
2004, 15(8): 935-938
[Abstract](182) [FullText HTML] [PDF 1148KB](0)
A new method to separate diazepam, nitrazepam, estazolam, alprazolam was established on both C18 and C8 CEC columns.The influence of separation voltage, Tris concentration, column temperature and the percentage of acetonitrile on the resolution and retention behavior of four benzodiazepines was investigated.The results showed that the percentage of acetonitrile had the largest effect on the resolution and retention behavior of the four benzodiazepines.Other separation conditions had also effects on the resolution and retention behavior, but smaller than the concentration of acetonitrile.Optimum separation conditions were obtained to separate four benzodiazepines on C18 and C8 CEC columns.
Study of Immunoassay Methods for Recombinant Human Erythropoietin (rhEPO) Using Competitive ELISA
Jin YAN , Jie Bo MI , Wen Bao CHANG
2004, 15(8): 939-942
[Abstract](178) [FullText HTML] [PDF 1322KB](0)
Two different immunoassay methods, competitive indirect enzyme-linked immuno-sorbent assay (CI-ELISA) and amplificative competitive indirect ELISA (ACI-ELISA) using biotin-avidin complex system were studied to detect rhEPO.The linear ranges were 50-20000 ng/mL and 10-50000 ng/mL for CI-ELISA and ACI-ELISA, respectively.The low detection limits of CI-ELISA and ACI-ELISA were 62.8 ng/mL and 8.5 ng/mL, respectively.
Production of Polyclonal Antibody of Morphine and Determination of Morphine in Urine by Capillary Electrophoresis Immunoassay with Laser-induced Fluorescence Detection
Jian Qiu MI , Xiao Hua QI , Xin Xiang ZHANG , Wen Bao CHANG
2004, 15(8): 943-946
[Abstract](183) [FullText HTML] [PDF 1155KB](0)
N-Conjugated antigen was synthesized and polyclonal antibody with high specificity was obtained from immunizing animals.With this polyclonal antibody, a rapid and efficient CEIA-LIF method was developed to determine the free morphine in urine of abusers.The detection limit was calculated to be 40 ng/mL.Simulated urine samples were analyzed with good recoveries, which showed the feasibility of its application in specific morphine determination in urine of morphine abusers.
Separation of Aniline Derivatives by Micellar Electrokinetic Capillary Chromatography
Jun LI , Zhuo Bin YUAN
2004, 15(8): 947-950
[Abstract](185) [FullText HTML] [PDF 1283KB](1)
A micellar electrokinetic capillary chromatography (MECC) was developed for the determination of aniline and 6 substituted anilines.The seven components were separated within 25 min in the buffer solution of 40 mmol/L sodium borate and 100 mmol/L SDS.It was found that the separation was dependent on operating voltage, pH value, borate and SDS concentrations.The analytical performance was examined in terms of linear response and reproducibility.Wastewater was determined by the established method.
A New Benzofuran Derivative from the Bark of Mulberry Tree
Sheng Jun DAI , Zhi Bo MA , Shuai LI , Ruo Yun CHEN , De Quan YU
2004, 15(8): 951-953
[Abstract](185) [FullText HTML] [PDF 917KB](2)
From the EtOH extract of the barks of Morus macroura Miq, a new benzofuran derivative, macrourin D 1, together with four known benzofuran derivatives, macrourin B 2, 2-(3, 5-dihydroxyphenyl)-5, 6-dihydroxybenzofuran 3, moracin M 4, and mulberroside C 5 were isolated, and their structures were determined on the basis of spectroscopic evidence and chemical correlation with known compounds.
Synthesis and Anion Recognition of a Novel Heterocyclic Organotin Complex
Li Xin ZHANG , Gui Zhi LI , Zhi Qiang LI
2004, 15(8): 954-956
[Abstract](299) [FullText HTML] [PDF 1078KB](0)
A novel heterocyclic hexacoordinate organotin(Ⅳ) complex, bis(O-vanillin)-semi ethylenediamino dibenzyltin (VEDBT) was synthesized by the reaction of dibenzyltin dichloride with bis(O-vanillin)-semiethyenediamine, its structure has been characterized by spectral methods.The electrodes using VEDBT as a neutral carrier show high selectivity for salicylate anions.
The Research on the Stability of TiO2,MoO3,PEO Doped Four-member Tungstic Acid Sols
Kai RAO , Xiang Kai FU , Xiao Ping RAO
2004, 15(8): 957-960
[Abstract](176) [FullText HTML] [PDF 1494KB](0)
The TiO2, MoO3, PEO doped four-member tungstic acid sols were prepared for the first time.The stability of different doped content sols were investigated and optimized with rotational viscometer.The four-member doped tungstic acid sol was very stable which could be stored more than two months at room temperature.The WO3 electrochromic film prepared from this doped four-member tungstic acid sol had excellent performance and longevity of service.
Comparative Study on the Inclusion Interaction between meso-Tetrakis (4-N-ethylpyridiniurmyl) porphyrin and β-Cyclodextrin Derivatives
Xi Liang GUO , Shao Min SHUANG , Jian Bin CHAO , Du Xin LI
2004, 15(8): 961-964
[Abstract](178) [FullText HTML] [PDF 1230KB](0)
The interaction of β-cyclodextrin (β-CD) and the modified cyclodextrins, hydroxy propyl-(-cyclodextrin (HP-β-CD), sulfobutylether-β-cyclodextrin (SBE-β-CD) and synthesized meso-tetrakis(4-N-ethylpyridiniurmyl)porphyrin (TEPyP) in aqueous solution has been studied by spectroscopic methods systematically.A significant change in fluorescence and absorption properties has been observed in the presence of β-CD, HP-β-CD and SBE-β-CD.The stoichiometry and formation constants have been determined by the steady-state fluorescence technique.The results showed that the β-CD derivatives were prior to the native β-CD and the hydrogen bonding and static electric forces played important roles in the formation of the inclusion complexes.The conformation was further confirmed by NMR spectroscopy.
Synthesis of Two Novel Rhenium (Ⅰ) Bipyridyl Photosensitive Dyes
Shi Guo SUN , Xiao Jun PENG , Ming Wen FAN , Yong Qian XU , Lei SHI , Li Cheng SUN
2004, 15(8): 965-968
[Abstract](263) [FullText HTML] [PDF 1520KB](0)
Two novel rhenium(Ⅰ) 2,2'-bipyridyl complexes,[(4,4'-di-COOEt-bipy) Re(CO)3 (NCCH3)PF6] and[(4,4'-di-COOEt-bipy) Re (CO)3 (NCS)], a model complex[(4,4'-di-COOEt-bipy) Re (CO)3 (pyridine)PF6], were synthesized.Their ground state electronic spectra and emission spectra were measured in acetonitrile.The MLCT absorption maximum of the complex exhibited a considerable red shift as the ligand changed from pyridine to CNCH3, or SCN.
A Convenient Synthesis and Properties of Ru (bpy)2[bpy (CO2H)-(CO2Et)](PF6)2 Photosensitive Dye
Shi Guo SUN , Xiao Jun PENG , Yong Qian XU , Lei SHI , Zhen GUO , Li Cheng SUN
2004, 15(8): 969-972
[Abstract](192) [FullText HTML] [PDF 1375KB](1)
A novel Ru(Ⅱ) tris-bipyridyl complex, Ru(bpy)2[bpy(CO2H)(CO2Et)] [PF6]2 is prepared in a simple and convenient process.It will be an alternative of Ru(bpy)2bpy(CO2Et)2(PF6)2 to be used in solar cells as photosensitive dyes.
Synthesis of Three Novel Chiral Binuclear Mn (Ⅲ)-Schiff-base Complexes and the Application in Asymmetric Epoxidation of trans-Stilbene
Yang SUN , Ning TANG , Xin Wen LIU , Wei Sheng LIU
2004, 15(8): 973-976
[Abstract](183) [FullText HTML] [PDF 1358KB](0)
Three novel chiral binuclear Mn(Ⅲ)-Schiff-base complexes have been synthesized and the application of these complexes in the asymmetric epoxidation of trans-stilbene is described, catalytic mechanism is also discussed briefly.
Effect of Different Dopant in the Mo-V-Te-O Catalyst on the Performance of Selective Oxidation Propane to Acrolein
Hua Chang JIANG , Wei Min LU , Hui Lin WAN
2004, 15(8): 977-980
[Abstract](172) [FullText HTML] [PDF 1328KB](0)
Several Mo-V-Te-O mixed metal oxides catalysts with different dopant were prepared and used for catalytic oxidation propane to acrolein.It was revealed that the addition of P could greatly improve the performance of the Mo-V-Te-O catalyst.The catalysts were examined by XRD and H2-TPR.The XRD characteristic of the Mo-V-Te-P-O showed that the addition of P could aggrandize the (V0.07Mo0.93)5O14 phase.H2-TPR illuminated that the MoV0.3Te0.23P0.15On catalyst took on the best redox ability.
Identification of Different Cobalt Nucleation on Glassy Carbon
Min GU , Fang Zu YANG , Ling HUANG , Shi Bing YAO , Shao Min ZHOU
2004, 15(8): 981-984
[Abstract](187) [FullText HTML] [PDF 1251KB](1)
The nucleation mechanisms of cobalt from sulfate solutions were studied by utilizing the electrochemical technique, chronoamperometry.It was found that the recorded current-time transients introduced from 1.0 mol/L CoSO4 solution were complexes with unusual shapes.All characteristic features were identified as separate process.The instantaneous or progressive nucleation with 2D or 3D growth exists during the cobalt deposition, depending on the applied potentials.
The New-generation of Green Surfactant (Alkylpolyglucoside) as an Inhibitor to the Corrosion of 907 Steel in Seawater
Min DU , Rong Jie GAO , Ping GONG , Qing Zhang WANG
2004, 15(8): 985-988
[Abstract](167) [FullText HTML] [PDF 1500KB](0)
Weight-loss trials and potentiodynamic polarization curves have been used to study the inhibitive properties of alkylpolyglucoside (APG) towards the 907 steel in seawater.The inhibition was different, if the length of alkyl chain APG was different.As the result, calcium gluconate, zinc sulfate and APG can protect 907 steel from being corrupted in static seawater.The compound corrosion inhibitor was found to control both the anodic process and the cathodic process.
The Adsorption of NOx on Magnesium Aluminium Hydrotalcite
Zhe Ming NI , Wei Hua YU , Shao Fen ZHAO , Zhong Hua GE
2004, 15(8): 989-992
[Abstract](284) [FullText HTML] [PDF 1315KB](0)
Magnesium aluminium hydrotalcite (Mg-Al-HT) with molar ratio of Mg-to-Al of 3 to 1 was prepared and characterized by X-ray diffraction (XRD) and infrared spectra (IR).The performances of Mg-Al-HT for the adsorption and desorption of NOx were studied.The results indicated that the adsorption capacity of the hydrotalcite for NOx was 1398.2 mg/g, and it was higher than the acticarbon's.The adsorption capacities depended on adsorption time and temperature.Mg-Al-HT could be regenerated by thermal decomposition, and the adsorption efficiency had not changed markedly after three cycles.
A Novel Approach for the Surface Modification of Polymeric Membrane with Phospholipid Polymer
Qing Wen DAI , Zhi Kang XU , Jian WU
2004, 15(8): 993-996
[Abstract](281) [FullText HTML] [PDF 1568KB](0)
A new economic and convenient method to modify the surface of microporous polypropylene (PP) membranes with phospholipid polymer was given.The process included the photo-irradiated graft polymerization of N,N-dimethylaminoethyl methacrylate (DMAEMA) and the ring-opening reaction of the grafted polyDMAEMA with 2-alkyloxy-2-oxide-1,3,2-dioxo-phospholanes (AOP).Four AOPs, whose alkyloxy groups consisted of dodecyl, tetradecyl, hexadecyl and octadecyl moieties, were used to convert the grafted polyDMAEMA to phospholipid polymers.FT-IR spectra confirmed the chemical change of membrane surface.Platelets adhesion experiment indicated that PP membrane with excellent blood compatible surface could be fabricated by this method.
DNA Nano-netting Intertexture on Carbon Electrodes
Xiang Qin LIN , Xiao Hua JIANG , Li Ping LU
2004, 15(8): 997-1000
[Abstract](181) [FullText HTML] [PDF 1478KB](0)
Native calf thymus double stranded DNA (ct-dsDNA) is successfully immobilized from solution onto carbon substrates by covalent linkages under an optimized deposition potential of 1.8±0.3 V vs.50 mmol/L NaCl-Ag/AgCl.The long chain DNA fabricates a layer of well conductive nano-netting intertexture, which is stable in pH 14 alkaline solution and in boiling water.The ct-dsDNA modified carbon fiber disk electrode shows two to three orders of magnitude enlarged electrode effective surface area and similarly enlarged voltammetric responses to Co(phen)33+ and dopamine.Thermal dissociated single stranded ct-DNA can also lead to similar result.This modified electrode will find wide applications in the fields of DNA-based electrochemical biosensors.
A Novel Method for Preparing Polyurethane Based Conductive Composites with Low Percolation Threshold
Ji Wen HU , Ming Wei LI , Ming Qiu ZHANG , Gen Shui CHENG , Min Zhi RONG
2004, 15(8): 1001-1004
[Abstract](278) [FullText HTML] [PDF 1616KB](0)
A novel method for preparing conductive carbon black filled polymer composites with low percolation threshold from polyurethane emulsion are reported in this paper.The experimental results indicate that with a rise in carbon black concentration the insulator-conductor transition in the emulsion blended composites occurs at 0.8-1.4vol%.In contrast, the solution blended composites exhibit drastic increase in conductivity at conducting filler fraction as high as 12.3-13.3vol%.It is demonstrated that the composites microstructure rather than chemical structure of the matrix polymer predominantly determines the electrical conduction performance of the composites.
Preparation of Silver Nanoshells on Silica Particles by a Simple Two-step Process
Yu ZHANG , Ming MA , Ning GU , Ling XU , Kun Ji CHEN
2004, 15(8): 1005-1008
[Abstract](287) [FullText HTML] [PDF 1287KB](0)
A simple two-step method was developed to prepare silver nanoshells coated on silica paticles.The method involves two steps:concentration of reaction precursor (AgNO3) on particle surfaces and subsequent reduction by formaldehyde.The obtained composite particles were characterized by TEM, ED, and SEM-EDS measurements.The results show that the silver nanoshell is coated on silica particle surface in the form of a polycrystalline (cubic structure) layer with average thickness of 20 nm and weight percentage of 19%.
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