2002 Volume 13 Issue 5

Michael Addition Reaction without Catalyst: The Synthesis of 2-Amino-5, 6, 7, 8-tetrahydro-5-oxo-4-aryl-7, 7-dimethyl- 4H-benzo-[b]-pyran Derivatives
Shu Jiang TU , Xiao Hong LIU , Heng Jun MA , Da Qing SHI , Fang LIU
2002, 13(5): 393-395
[Abstract](213) [FullText HTML] [PDF 1093KB](0)
Abstract:
Aseries of tetrahydrobenzo-[b]-pyran derivative was synthesized by the reaction of arylmethylene malononitrile or arylmethylene cyanoacetate with dimedone in ethylene glycol at 80℃ without catalyst. The structures of the two products were characterized by X-ray diffraction.
Samarium(Ⅱ) Diiodide Induced Polarity Inversion of π-Allyl Palladium Complexes: The Formation of Allylic Selenides
Xin Jian ZHAO , Hua Rong ZHAO , Xian HUANG
2002, 13(5): 396-397
[Abstract](211) [FullText HTML] [PDF 704KB](2)
Abstract:
Allylic acetates were reduced with Pd(0)-SmI2 in the presence of ArSeBr to form corresponding allylic selenides in good yields.
Investigation of Isomerization of 2-Seleno-l, 3,2-diazaphospholidine Derivatives
Sheng Lou DENG , Ru Yu CHEN , Dong Zhi LIU
2002, 13(5): 398-401
[Abstract](197) [FullText HTML] [PDF 1173KB](0)
Abstract:
For the first time the isomerization of 1, 3, 2-diazaphospholidine-2-selenide derivatives in refluxing benzene in the presence of trace water was observed. The structures of isomerized products were determined by IR, 1H NMR, 31P NMR, elemental analysis and X-ray crystallography. The mechanism of isomerization was also proposed.
A New Synthetic Method for N-Substituted Selenoamides
Hua Rong ZHAO
2002, 13(5): 402-404
[Abstract](190) [FullText HTML] [PDF 1115KB](1)
Abstract:
Bcnzotriazolc, aldehydes and primary selenoamides read together with elimination of water to form 1:1:1 adducts which arc rcduccd smoothly by NaBH4 to give the N-substituted selenoamides in good yield.
Cobalt(Ⅰ) Catalyzed Reaction of Benzaldehydes with Functionalized Benzylic Zinc Halides
Jin Xian WANG , Ying FU , Yu Lai HU
2002, 13(5): 405-406
[Abstract](191) [FullText HTML] [PDF 778KB](0)
Abstract:
Funclionalizcd bcnzylic zinc halides rcactcd with bcnzaldehydcs in the prcscncc of Lewis acid Mc3SiCl giving high yields of trans-vstilbcncs under the catalysis of Co(PPh3)3Cl.
A Facile Synthesis of Benzoxazolyl Cyclopropanes
Jian Guo SHAO , Pei Yu WANG , Ming ZHENG , Qi ZHONG
2002, 13(5): 407-409
[Abstract](187) [FullText HTML] [PDF 894KB](0)
Abstract:
2'-Benzoxazolyl substituted cyclopropane derivatives were synthesized in the yield of 73-89% from the reaction of telluronium ylides with chalcones.
A Convenient Method of Polyfluoroalkyl-lactonization
Xiao Wei ZOU , Fan Hong WU
2002, 13(5): 410-411
[Abstract](193) [FullText HTML] [PDF 663KB](0)
Abstract:
A novel synthesis of polyfluoroalkyl substituted γ-butyrolactones from the reaction of polyfluoroalkyl iodides with 4-pentenoic acid initiated with sodium dithionite was realized in good yields.
Syntheses of 3,7-disubstitrted 1,4-benzepin-2-one
Sheng Biao WAN , Zong Ru GUO
2002, 13(5): 412-415
[Abstract](197) [FullText HTML] [PDF 1218KB](0)
Abstract:
A series of 3-methoxycarbonylpropoxy-7-(imidazol-4-ylpropinamide)-1, 3-dihydrogen-1-methyl-5-phenyl-2H-1, 4-benzodiazepin-2-ones, as farnesyltransferase(Ftase) inhibitors, were synthesized. The preparation of the key intermediate, 7-amino-3-methoxycabonylpropoxy-1- methyl-5-phenyl-2H-1,4-benzodiazepin-2-one, was improved.
Enzymatic regioselective symthesis of vinthesis of vinyl lactose ester and its chemical polymerization
Qi WU , Jian Yue FENG , Chen Guo FENG , De Shui LU , Xian Fu LIN
2002, 13(5): 416-419
[Abstract](174) [FullText HTML] [PDF 1440KB](0)
Abstract:
Transesterification reaction of lactose with divinyladipate in pyridine catalyzed by an alkaline protease from Bacillus subtilis at 50℃ for 3 days gave 6'-O-vinyladipoyl-lactose (yield 35%). Poly(6'-O-vinyladipoyl-lactose) with Mn=21,200, Mw=32,900, Mw/Mn=1.56 could be obtained by chemical polymerization. Poly(vinyl alcohol) containing lactose branch was biodegradable. After 6 days in aqueous buffer (PH 7), this alkaline protease could degrade the polymer to an Mn of ca. 2100, Mw/Mn=2.56.
Dendritic Macroinitiator for the Ring-Opening Polymerization of γ-Benzyl L-Glutamate N-Carboxyanhydride
You Liang ZHAO , Chuan Fu CHEN , Fu XI
2002, 13(5): 420-421
[Abstract](175) [FullText HTML] [PDF 746KB](0)
Abstract:
By using OH-terminated polyarylether dendrimer and N-Fmoc-glycine as raw materials, the dendritic polyarylether 2-aminoacetate (G3-NH2) was synthesized via two step reactions. G3-NH2 as a macroinitiator for the ring-opening polymerization of γ-benzyl L-glutamate N-carboxyanhydride was investigated. It is found that the resulting copolymers possessed relatively high molecular weight and narrow molecular weight distribution (1.12< Mw/Mn<1.28).
Novel Bipolar Conjugated Polymer Containing Both Triphenylamine and Oxadizole Units
Guang WANG , Ze LIU , Li Xiang WANG , Xia Bin JING , Fo Song WANG
2002, 13(5): 422-425
[Abstract](179) [FullText HTML] [PDF 1553KB](0)
Abstract:
A novel bipolar conjugated polymer containing triphenylamine and 1, 3, 4-oxadiazole units was synthesized by Suzuki reaction. Its structure and properties were characterized by NMR, IR, UV-Vis, PL spectroscopy and electrochemical measurement. The photoluminescent spectroscopy and cyclic voltammograms measurement demonstrated that the resulting polymer shows blue emission (477 nm) and possesses both electron and hole-transporting property
A New Benzylisoquinoline Alkaloid from Sabia parviflora
Jin CHEN , Bin CHEN , Jun TIAN , Feng E WU
2002, 13(5): 426-427
[Abstract](185) [FullText HTML] [PDF 613KB](0)
Abstract:
A new benzylisoquinoline alkaloid, 1, 2, 3, 4-tetrahydro-5-hydroxyl-8-methoxyl-2- methyl-4'-methoxyl-benzylisoquinoline, was isolated from the arial parts of Sabia parviflora. Its structure was established on the basis of spectral analysis.
A Minor New Flavone from Scutellaria baicalensis Georgi
Hong Yan WANG , , Sui Xu XU , Ying Jie CHEN , J. Tze Fei WONG , Hong XUE
2002, 13(5): 428-429
[Abstract](182) [FullText HTML] [PDF 619KB](0)
Abstract:
A new flavone, 6, 2'-dihydroxy-5, 7, 8, 6'-tetramethoxyflavone, was isolated from the roots of Scutellaria baicalensis. Its structure was established on the basis of spectral evidences.
A New Monoterpene Glycoside from Paeonia veitchii
Shao Hua WU , Xiao Dong LUO , Yun Bao MA , Xiao Jiang HAO , Da Gang WU
2002, 13(5): 430-431
[Abstract](182) [FullText HTML] [PDF 682KB](0)
Abstract:
A new monoterpene glycoside, acetoxypaeoniflorin, was isolated from the root cortex of Paeonia veitchii Lynch.. The structure was elucidated by spectral methods.
Two new acyclic diterpene-y-lactones from the leaves of Salix matsudana
Jin Xin WANG , Shang Zhen ZHENG , Tong SHEN , Xu Wei SHEN , Ying LI
2002, 13(5): 432-435
[Abstract](176) [FullText HTML] [PDF 1251KB](0)
Abstract:
Two new acyclic diterpene-γ-lactones named hanliuine Ⅲ (1) and hanliuine Ⅳ (2) were isolated from leaves of Salix matsudana(Chinese name "hanliu"). Their structures were deduced from spectral data.
Ni2+-PAA Adsorbent for Purifying 6His-OmpTS Recombinant Protein
Qing Bing ZENG , Qiao Zhen YE , Jia Rui XU , Ruo Wen FU
2002, 13(5): 436-439
[Abstract](180) [FullText HTML] [PDF 1514KB](0)
Abstract:
Functional Ni2+-polyacrylic acid (Ni2+-PAA) adsorbent has been prepared for metal chelate affinity chromatography. DNA elements coding for adjacent histidines were fused to the Aeromonas hydrophila ompTS gene. Subsequent expression in E. coli resulted in the production of hybrid protein 6His-OmpTS that could be purified by Ni2+-PAA affinity chromatography.
Determination of Roxithromycin Tablets by Capillary Electrophoresis Employing Non-aqueous Media with Square-wave Amperometric Detection
Na LI , Tian Yao XIE , Jin Yuan MO
2002, 13(5): 440-441
[Abstract](189) [FullText HTML] [PDF 999KB](0)
Abstract:
A new method of determination for roxithromycin tablets by non-aqueous capillary electrophoresis (NACE) with square-wave amperometric detection was carried out. Several parameters affecting the NACE-AD determination were studied. The data was modified by spline wavelet least square (SWLS). The method is simple, rapid and highly reliable for routine analysis.
The Standard Association Constant of Ion Pair [GaCl]2+in the System of HCl+GaCl3+H2O
Jia Zhen YANG , Ru Bo ZHANG
2002, 13(5): 442-443
[Abstract](175) [FullText HTML] [PDF 52KB](0)
Abstract:
The standard association constants of ionic pair [GaCl]2+, Kas, were determined by emf(electromotive force) method at 278.15 to 318.15 K. The thermodynamic quantities for the ionic association process were calculated and it was pointed that the association entropy is driving force to form the ionic pair.
Fine Structure of Hydrogen Bond in Cholic Acid Revealed by 2DIR Spectroscopy
Bao Gui HUANG , Yi Zhuang XU , , Shi Fu WENG , Wen Xiu SUN , Jin Guang WU , Duan Fu XU , Guang Xian XU
2002, 13(5): 444-447
[Abstract](197) [FullText HTML] [PDF 1673KB](1)
Abstract:
Based on cryogenic FT-IR spectroscopic studies of hydrogen bonds in cholic acid, two-dimensional FT-IR spectroscopy was applied to enhance our understanding of the hydrogen bonds of cholic acid. Fine spectral structures were revealed by asynchronous 2D FT-IR spectra. The co-relationship among various bands was discussed according to the synchronous 2D FT-IR spectrum.
Dynamic Behavior and Mass Transport in Polyacrylic Acid Gel by Dynamic Light Scattering
Ju ZUO , Jian Feng HUANG , Ying Li AN , Fang Xing LI , Chang Ying ZHU , Li LIU , Zhi Guang ZHANG , Bing Lin HE
2002, 13(5): 448-451
[Abstract](191) [FullText HTML] [PDF 1493KB](1)
Abstract:
Dynamic behaviors on polyacrylic acid (PAA) gels and mass (small molecules) transports in the gels have been studied mainly by dynamic light scattering (DLS). The cross-linking degree (fc), monomer concentration (Cm) and temperature of the gels have significant influences on its dynamic behavior and mass transport in the gels. The increase of fc leads to decrease of the mesh sizes of the gels, thus the obstacle of the gels for mass transport is increased. As a result, small molecular diffusion Dk in the gels is decreased. So even if for small molecules, the Dk also is influenced.
Two-photon Up-conversion Luminescent Properties of HMASPS and HEASPS in Three Different Polymer Matrices
Yan REN , Xiao Qiang YU , Dong WANG , Guang Yong ZHOU , Zhi Qiang LIU , Yu Fang ZHOU , Xian ZHAO , Zong Shu SHAO , Ji Yang WANG , Min Hua JIANG
2002, 13(5): 452-455
[Abstract](189) [FullText HTML] [PDF 1230KB](1)
Abstract:
Three dye-doped polymer rods in different matrices were synthesized in which weak hydrogen bond, strong hydrogen bond and covalent bond existed between the dye and the polymer chain. And the two-photon up-conversion luminescent properties of HMASPS and HEASPS1
Effect of Thermal History on Rheological Properties of Partially Hydrolyzed Polyacrylamide/Anionic Surfactant SDS Complex Systems
Huai Tian BU , Zhen Zhong YANG , Li HUANG
2002, 13(5): 456-459
[Abstract](180) [FullText HTML] [PDF 1797KB](0)
Abstract:
The effects of thermal history on the rheological properties of partially hydrolyzed polyacrylamide/sodium dodecyl sulfate complex aqueous solutions have been studied using both steady shear and dynamic temperature sweep characterizations. An abnormal rheological behavior was found that dynamic moduli of the aqueous solutions increased, while the viscosity decreased after thermal treatment, which could help to gain insight into the micro-phase evolution of the polymer/surfactant complex aqueous solutions and its dependence on temperature.
Preparation and Photochromic Behavior of Novel Hybrid Inorganic-Organic Thin Film
Wei FENG , Tie Rui ZHANG , Yan LIU , Ran LU , Ying Ying ZHAO , Jian Nian YAO
2002, 13(5): 460-463
[Abstract](181) [FullText HTML] [PDF 1479KB](0)
Abstract:
A novel photochromic complex comprising of Keggin type tungstophosphate acid (PW12) and polyacrylamide (PAM) was prepared. FT-IR results showed that the Keggin geometry of PW12 was still preserved inside the composite, and a charge-transfer bridge was built between PW12 and PAM via hydrogen bond. AFM images indicated that surface topography of polymer matrix changed after adding PW12. Under UV irradiation, the film was reduced photochemically to yield a blue species, which was reversible in the present of oxygen in polymeric network.
A Transparent Thin Film with Hexagonal Mesostructure Containing Rhodamine 6G
Yun Feng YAO , Mai Sheng ZHANG , Yan Sheng YANG , Qiang SU , , Hong Jie ZHANG
2002, 13(5): 464-467
[Abstract](162) [FullText HTML] [PDF 1652KB](1)
Abstract:
A transparent thin film was prepared by depositing the sol-gel mixture for the synthesis of MCM-41 mesoporous molecular sieve doped with rhodamine 6G (R6G) dye on glass substrates. The film of silica-surfactant-R6G materials, which was identified to possess hexagonally ordered mesostructure, was composed of nanocrystallites about 35 nm in diameter and 1-10(m in thickness. Cleanness of the substrates, concentration of the sol-gel mixture and rate of evaporation of the solvent were the key factors affecting transparency and homogeneity of the film. Moreover, optical change and lack in dye aggregation were observed to the R6G-functionalized MCM-41 thin film in contrast with that in ethanol solution.
Polyether-phosphinite for One-phase Catalysis Coupled with Two-phase Separation
Yan Hua WANG , Xiao Zhong LIU , Cui Ying JIA , Zi Lin JIN
2002, 13(5): 468-471
[Abstract](167) [FullText HTML] [PDF 1270KB](0)
Abstract:
Polyether moiety was introduced to the phosphinite and the phosphinite modified rhodium complex formed in situ was highly active in the hydroformylation of higher olefins in organic monophase system. After reaction, on cooling to room temperature, the catalyst could precipitate out from organic phase and was easily separated by decantation and reused six times without obvious decreasing in activity
Performance of Pt-TiO2 Electrocatalyst for CO Oxidation in the Electrochemical Gas Sensor
Chun Bo YU , Hui YANG , Tian Hong LU , Yu Jiang WANG , Kai Feng HUA , Wei XING
2002, 13(5): 472-473
[Abstract](160) [FullText HTML] [PDF 716KB](0)
Abstract:
It is reported for the first time that the Pt/TiO2 electrocatalyst was successfully used for the electrocatalytic oxidation of CO in the electrochemical gas sensor with a controlled potential mode. The stability of electrocatalytic activity of the Pt-TiO2 electrocatalyst for the CO oxidation is better than that of Pt.
Synthesis of a Chain Aluminophosphate Containing Racemic 1, 2-Diaminopropane
Wei CHEN , Yu Sheng JIANG , Hua HUO , Hong Ming YUAN , Jie Sheng CHEN
2002, 13(5): 474-477
[Abstract](144) [FullText HTML] [PDF 1403KB](0)
Abstract:
A one-dimensional chain aluminophosphate C1.5H7.5N1.5Al0.5PO4 containing diprotonated racemic 1, 2-diaminopropane cations was synthesized from an alcoholic system. The compound consists of infinite inorganic [AlP2O8] chains of alternately connected AlO4 and PO2(=O)2 tetrahedral units and the racemic template molecules. The macroanionic chains contain corner-shared double four-membered rings.
Preparation of Pt/C Catalyst with Solid Phase Reaction Method
Ya Wen TANG , Hui YANG , Wei XING , Tian Hong LU
2002, 13(5): 478-479
[Abstract](164) [FullText HTML] [PDF 794KB](0)
Abstract:
The Pt/C catalyst was prepared with solid phase reaction method (Pt/C(S)) for the first time. Its performances were compared with that prepared by the traditional liquid phase reaction method. The results demonstrate that the electrocatalytic activity of Pt/C catalyst with solid phase reaction method for methanol oxidation is higher than that with liquid phase reaction method. XRD and TEM measurements indicate that the Pt/C(S) possesses low crystalline extent and small particle size.
Simultaneous Removal of Surfactant Template from MCM-41 and Implantation of Transition Metal Complexes into Mesopores with Supercritical Fluid
Xiao Bing LU , Wen Hua ZHANG , Ren HE
2002, 13(5): 480-483
[Abstract](150) [FullText HTML] [PDF 1569KB](0)
Abstract:
The simultaneous removal of up to 92% of the surfactant template and chemical implantation of transition metal complexes into mesopores has been successfully achieved by treating as-synthesized pure siliceous MCM-41 with supercritical CO2 modified with CH2Cl2/MeOH mixture, resulting in the formation of functionalized material with uniform pore structure.
Atomic Force Microscopy Studies on the Chemical Treatment of Nanocrystalline Porous TiO2 Films
Yuan LIN , Feng Zhi JIANG , Jing Bo ZHANG , Yan Lin SONG , Lei JIANG , Xu Rui XIAO
2002, 13(5): 484-486
[Abstract](151) [FullText HTML] [PDF 1143KB](0)
Abstract:
AFM has been utilized to study the surface topography and the local conductivity of nanocrystalline TiO2 films. Improving the local conductivity by Ti(iso-C3H7O)4 treatment is characterized by quantitative analysis of the simultaneous current image. The mechanism of Ti(iso C3H7O)4 treatment is discussed.
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