2004 Volume 15 Issue 9

Solid-phase Synthesis of Unsaturated β-Dicarbonyl Compounds from Polymer-supported 4-(Phenylseleno) morpholine
Xiao Ling LIU , Xing Cong WANG , Shou Ri SHENG , Xian HUANG
2004, 15(9): 1009-1010
[Abstract](194) [FullText HTML] [PDF 601KB](0)
The solid-phase synthesis of unsaturated β-dicarbonyl compounds has been reported.
Synthesis of Novel Antifungal Triazole Compounds
Yong CHU , Ming Xia XU , Ding LU
2004, 15(9): 1011-1014
[Abstract](196) [FullText HTML] [PDF 1471KB](0)
Based on our previous studies of 3D-QSAR, 38 novel objective compounds belonging to 4 series were designed and successfully synthesized directed by the idea of reconstructing the structure of non-pharmacophores while reserving essential ones in triazoles. In vitro pilot studies on their antifungal activities showed that most compounds have inhibitory effects on C.albicans and some inhibit S.cerevisiae also. The effects on C.albicans of 5 compounds are more potent than or equal to that of fluconazole or itraconazole.
Asymmetric Induction of Chiral 1,1'-Bis (oxazolinyl) ferrocenes as Ligands in Metal-Catalyzed Cyclopropanation and Diels-Alder Reactions
Zhen QIAO , Xue Yan SHI , Qing Hua BIAN , Shi Cong HOU , Min WANG
2004, 15(9): 1015-1018
[Abstract](196) [FullText HTML] [PDF 1329KB](0)
Four chiral 1,1'-bis(oxazolinyl)ferrocenes(1a-1d) have been prepared and used as ligands in the copper catalyzed asymmetric cyclopropanation of styrene with ethyl diazoacetate (EDA) and the magnesium catalyzed Diels-Alder reaction between 3-acryloyl-2-oxazolidinone and cyclopentadiene. Enantioselectivities up to 24% and 41%, respectively, for cyclopropanation and Diels-Alder reaction were observed.
Synthesis of Calix[4]resorcinarene Amide Derivatives
Chao Guo YAN , Yun GE
2004, 15(9): 1019-1021
[Abstract](206) [FullText HTML] [PDF 1062KB](5)
Three different synthetic routes were developed to introduce carbamoyloxy functional groups at the upper periphery of two calix[4]resorcinarenes. By treating activated esters 2a-b with excess corresponding amine such as 3-(dimethylamino)propylamine 3, α-phenethylamine 4 and triethylenetetramine 5, six amide derivatives 6a~8b were obtained in high yield (Route 1). The pyridine-linked amide derivatives 9a-b were prepared by using acid chloride intermediate (Route 2). The amide derivatives 10a-b were obtained in moderate yields by direct alkylation of phenolic hydroxyl groups of 1a-b with N,N-dipropylchloroacetoamide in the presence of K2CO3/KI in acetone (Route 3).
Biphasic Catalytic (Hydroformylation of 1-Dodecene in Micellar System with Cationic Gemini Surfactants
Min LI , Bin XU , Hua CHEN , Hong Jie ZHENG , Xue Yuan HUANG , Yao Zhong LI , Xian Jun LI
2004, 15(9): 1022-1024
[Abstract](199) [FullText HTML] [PDF 1142KB](0)
The promotion effect of cationic gemini surfactants for the hydroformylation of 1-dodecene in the organic/aqueous biphasic catalytic system is reported. The hydroformylation reaction in the presence of gemini surfactant occurred with higher turnover frequency and higher selectivity for linear aldehyde than using conventional monomeric surfactant CTAB.
Synthesis of chiral N-ferrocenylmethylaminoalcohols and their applica-tion in enantioselective addition of diethylzinc to aldehydes
Jian Feng GE , Zong Xuan SHEN , Ya Wen ZHANG
2004, 15(9): 1025-1028
[Abstract](207) [FullText HTML] [PDF 1353KB](0)
Three chiral N-ferrocenylmethylaminoalcohols were synthesized from readily available natural L-valine, leucine and phenylanine, and used as chiral ligands in the enantioselective addition of diethylzinc to aldehydes.
A Facile and Efficient Oxidation of (,(-Unsaturated Alcohols with Manganese Dioxide in Ionic Liquids under Mild Conditions
Wei Liang BAO , Qiang WANG , Yun Fa ZHENG
2004, 15(9): 1029-1032
[Abstract](193) [FullText HTML] [PDF 1467KB](2)
The oxidation of α,β-unsaturated primary and secondary alcohols to corresponding aldehydes and ketones by manganese dioxide in ionic liquids as a safe recyclable and accelerative reaction medium under mild conditions are described. The rate of the oxidation reaction is faster and the yield is higher than that with conventional procedures.
An Unusual Formation of Cyclic Sulfite at C-4 and C-5 Positions of Taxane
Meng ZHANG , Da Li YIN , Ji Yu GUO , Xiao Tian LIANG
2004, 15(9): 1033-1035
[Abstract](191) [FullText HTML] [PDF 971KB](0)
An unusual formation of cyclic sulfite at C-4 and C-5 positions of taxane was accomplished by treatment of compound 1 with excess MeSO2Cl/Et3N and a possible mechanism was proposed.
First Total Synthesis of (±)-Aiphanol
Xiao Long WANG , Jian Peng FENG , Xin Gang XIE , Xiao Ping CAO , Xin Fu PAN
2004, 15(9): 1036-1038
[Abstract](207) [FullText HTML] [PDF 1067KB](0)
(±)-Aiphanol was first synthesized in which coupling reaction and Horner-Wittig reaction as the key steps.
Synthesis and Anti-influenza Virus Activity of Ethyl 6-Bromo-5-hydroxyindole-3-carboxylate Derivatives
Yan Fang ZHAO , Jin Hua DONG , Ping GONG
2004, 15(9): 1039-1042
[Abstract](186) [FullText HTML] [PDF 1454KB](0)
A series of ethyl 6-bromo-5-hydroxyindole-3-carboxylate derivatives were synthesized and their in vitro anti-influenza virus activity was evaluated. All the compounds were characterized by 1H NMR and MS.
Anodic Cyanation of 1-(1-Methoxycarbonyl ethyl) piperidine
Ping ZHAO , Ying Wu YIN
2004, 15(9): 1043-1046
[Abstract](774) [FullText HTML] [PDF 1234KB](1)
α-Aminonitriles were prepared efficiently from anodic cyanation of α-amino ester. The effect of different solvents and electrolytes was studied. The other byproducts were analyzed.
Polystyrene-supported Selenomethyl-sulfonates:Efficient Reagents for Stereocontrolled Synthesis of Substituted Vinyl Sulfones
Wei Ming XU , Lu Ling WU , Xian HUANG
2004, 15(9): 1047-1049
[Abstract](188) [FullText HTML] [PDF 875KB](0)
Polystyrene-supported selenomethyl-sulfonates have been prepared. These novel reagents were treated with LDA to produce selenium stabilized carbanions, which reacted with alkyl halide and epoxides, followed by selenoxide syn-elimination, to give E-vinyl sulfones and γ-hydroxy-substituted-E-vinyl sulfones respectively.
Study on the Novel Dicyanate Ester Resin Containing Naphthalene Unit
Hong Qiang YAN , Hong Yun PENG , Li JI , Guo Rong QI
2004, 15(9): 1050-1052
[Abstract](199) [FullText HTML] [PDF 893KB](0)
The novel dicyanate ester resin containing naphthalene unit (DNCY) was synthesized, and characterized by FT-IR, 1H-NMR, 13C-NMR and elemental analysis (EA).The thermal properties of DNCY resin was studied by thermal degradation analysis at a heating rate of 10 ℃/min-1 in N2 and air. The DNCY resin exhibited better thermal and thermal-oxidative stability than bisphenol A dicyanate (BACY) resin.
A Lignan Glucoside from Bupleurum scorzonerifolium
Li TAN , Bin WANG , Yu Ying ZHAO
2004, 15(9): 1053-1056
[Abstract](189) [FullText HTML] [PDF 1246KB](0)
A new lignanoside, saikolignanoside A, was isolated from the roots of Bupleurum scorzonerifolium. Its structure was determined as 3-methoxy-4-hydroxy-5-[(8'S)-3'-methoxy-4'-hydroxyphenylpropyl alcohol]-E-cinnamic alcohol-4-O-β-D-glucopyranoside by means of NMR and MS analysis, acid hydrolysis and optical data.
Two New Isoquinoline Alkaloids from Carduus crispus
Wei Dong XIE , Zhong Jian JIA
2004, 15(9): 1057-1059
[Abstract](194) [FullText HTML] [PDF 924KB](0)
Two new isoquinoline alkaloids:carcrisine A and B, have been isolated from the whole plant of Carduus crispus L.. Their structures were elucidated by chemical and spectroscopic methods.
Surface Confined Ionic Liquid-A New Stationary Phase for the Separation of Ephedrines in High-performance Liquid Chromatography
Shu Juan LIU , Feng ZHOU , Xiao Hua XIAO , Liang ZHAO , Xia LIU , Sheng Xiang JIANG
2004, 15(9): 1060-1062
[Abstract](195) [FullText HTML] [PDF 912KB](3)
In this article, a new and effective stationary phase based on ionic liquid modified silica is first reported and used for the separation of ephedrines in high-performance liquid chromatography (HPLC). The separation results indicate the high efficiency and reproducibility of the stationary phase. The electrostatic interaction, ion-exchange interaction between the solutes and the stationary phase are considered to attribute the effective separation. Moreover, the free silanols on the surface of the silica are effectively masked by the immobilized ionic liquid, a result of which is to decrease the non-specific absorption.
Separation of Biphenyl Nitrile Compounds by Microemulsion Electrokinetic Chromatography with Mixed Surfactants
Su Xuan GONG , Tao BO , Lan HUANG , Ke An LI , Hu Wei LIU
2004, 15(9): 1063-1066
[Abstract](189) [FullText HTML] [PDF 1553KB](0)
A mixture of nine biphenyl nitrile compounds with high hydrophobicity and similar structures was successfully separated by microemulsion electrokinetic chromatography (MEEKC) within 30 min. The buffer system contained 100 mmol/L sodium dodecyl sulfate (SDS), 80 mmol/L sodium cholate (SC), 0.81% heptane, 7.5% n-butanol, 10% acetonitrile and 10 mmol/L borate. The addition of SC, organic modifiers, sample preparation and temperature all showed remarkable effect on the separation. Meanwhile, the MEEKC method was briefly compared with micellar electrokinetic chromatography (MEKC) method.
Determination of Baicalin in Traditional Chinese Preparation by High Performance Liquid Chromatography with Chemiluminescence Detection
Er Bao LIU , Hong Qing WEI , Xiu Li ZHAO , Xiao Xia LI , Feng Xian JIANG
2004, 15(9): 1067-1070
[Abstract](200) [FullText HTML] [PDF 1298KB](0)
A new method for the determination of baicalin with HPLC-CL was developed. The method was based on the chemiluminescence reaction between KMnO4 and baicalin sensitized from HCHO. The linear range was 3.7×10-6~9.8×10-5 mol/L with detection limit of 1.7×10-6 mol/L and the relative standard deviation was 2.5% (Cs=6.6×10-5 mol/L, n=5). The method has been applied to the determination of baicalin in oral administration, injection, Scutellariae radix and granules with good results.
Analysis of the Aconitine Alkaloids in Chuanwu by Electrospray Ionization/Tandem Mass Spectrometry
Ai Min SUN , Hui LI , Zhi Ming HUANG , P. P. H. BUT , Xue Qin DING
2004, 15(9): 1071-1074
[Abstract](186) [FullText HTML] [PDF 1592KB](0)
An electrospray ionization/tandem mass spectrometric (ESI/MS/MS) method was developed for the simultaneous identification and analysis of three aconitine alkaloids[mesacontine (MA), hypaconitine (HA), and aconitine (A)] as intact molecules at low nanogram level in Chinese traditional medicine Chuanwu decoction as well as in human whole blood extract without chromatographic separation.
Thermokinetic Behaviour Degenerated from Limit Cycle Oscillation of Isothermal B-Z Reaction System due to Temperature Controlling of Heat Compensation Type
Wen Hua ZHANG , Jiu Li LUO
2004, 15(9): 1075-1078
[Abstract](182) [FullText HTML] [PDF 1304KB](0)
The thermokinetic behavior of the B-Z reaction system was influenced by both the chemical reaction-heat conduction coupling and the temperature undulation due to temperature controlling of heat compensation type. Quantitative research indicated that this kind of temperature fluctuation will lead to limit cycle degeneration and the periodic or quasi-periodic response behavior of the focus near a supercritical Hopf bifurcation.
Study of Interaction between Red-tide Toxin,Domoic Acid and Double-stranded DNA by Capillary Zone Electrophoresis
Da Zhi LI , Xin Ya HE , Hui WANG , Li SUN , Bing Cheng LIN
2004, 15(9): 1079-1082
[Abstract](188) [FullText HTML] [PDF 1128KB](0)
The interactions between amnesic red-tide toxin, domoic acid (DA) and 14mer double-stranded DNA (dsDNA with three kinds of sequences) were studied by capillary zone electrophoresis (CZE). For the dsDNA with a sequence of 5'-CCCCCTATACCCGC-3', the amount of free dsDNA decreases with the increase of added DA; and the signal of DA-dsDNA complex was observed. Meanwhile, the other two dsDNAs, 5'-(C)12GC-3' and 5'-(AT)7-3', the existence of DA could not lead to the change of dsDNA signal and indicated that there is no interaction between DA and these two dsDNAs.
The Stabilization Effect of Glutaraldehyde on the Spirulina platensis Phycobilisomes
Xi Ying ZHANG , Xiu Lan CHEN , Wei LIU , Yu Zhong ZHANG , Bai Cheng ZHOU
2004, 15(9): 1083-1086
[Abstract](189) [FullText HTML] [PDF 1327KB](0)
The spectral properties of the glutaraldehyde-treated phycobilisomes were studied. The results showed that glutaraldehyde was effective in preventing phycobilisomes from dilutioninduced dissociation and preserving the intra-phycobilisomes energy transfer.
Synthesis and Characterization of Novel Mercapto-end Ferrocenyl Derivatives with Schiff Base Linkage
Hai Feng SONG , Miao CHEN , Yong Min LIANG , Ling SHI , Guo Sheng HUANG
2004, 15(9): 1087-1090
[Abstract](185) [FullText HTML] [PDF 1494KB](0)
Novel ferrocenyl derivatives of p-(10-mercaptodecyloxy) benzal 4-ferrocenylaniline have been prepared and characterized by element analysis, 1HNMR, and FAB-MS. Cyclic voltammetry has been used to characterize the self-assembled monolayers formed from the compounds on the gold electrodes.
A Novel Method for Quantification of Circulating DNA in Serum by Capillary Zone Electrophoresis
Peng ZHANG , Ji Cun REN , Zuo Jun SHEN
2004, 15(9): 1091-1094
[Abstract](197) [FullText HTML] [PDF 1484KB](0)
In this paper, we first presented a novel method for quantification of circulating DNA in human serum based on capillary zone electrophoresis with laser-induced fluorescence detection (CZE-LIF). The serum was digested by proteinase to release free DNA, and then CZE-LIF system was used for the quantification of total circulating DNA. This method was successfully used to quantify the circulating DNA levels in sera from healthy individuals and certain cancer patients. We found the significantly elevated circulating DNA levels in certain prostate cancer patients. Our results demonstrated that CZE-LIF system has good linearity, excellent sensitivity (0.5 ng/mL DNA), satisfactory reproducibility (RSDs in one day and between days were both less than 5%) and reliability, and is well suitable to the quantification of the circulating DNA in human serum or plasma.
A Study of Heteropoly Complexes of Rare Earths as Catalyst Promoter in the Synthesis of Ethyl Acetate
Shui Yang HE , Ke PENG , Di ZHANG , Wang Ting WU , Gang Lin XUE , Qi Zhen SHI
2004, 15(9): 1095-1097
[Abstract](200) [FullText HTML] [PDF 877KB](0)
The capability of the synthesized heteropoly complexes of rare earths {K10[(O39W11Si) Ln(Gly)3Ln(SiW11O39)]·9H2O (Ln=La, Pr, Nd, Sm, Eu, Gd, Tb, Dy)} as the catalyst promoter in the synthesis of the ethyl acetate was studied. The results showed that the quantity of H2SO4 used for synthesizing the ethyl acetate can be reduced by 75% and the yield reached 98% at the optional condition.
Electropolymerization of O-Phenylenediamine in an Ionic Liquid
Yan Fang DU , Xi Min QI , Peng ZHAO , Jia Xing LU , Ming Yuan HE
2004, 15(9): 1098-1100
[Abstract](183) [FullText HTML] [PDF 1073KB](0)
Ionic liquid like 1-ethyl-3-methylimidazolium bromine ([EMIM]Br) has been used as electrolyte for the electropolymerization of O-phenylenediamine at glassy carbon electrode by cyclic voltammetry. It is found that poly (O-phenylenediamine) film modified electrode has favorable electrochemical activity in acid solution.
Effect of Addition of Cosurfactant on the Phase Behaviour of Oil-in-water Aminosilicone Oil Microemulsion
Zheng Hong LUO , Xiao Li ZHAN , Peng Yong YU
2004, 15(9): 1101-1104
[Abstract](188) [FullText HTML] [PDF 1688KB](0)
Stable and transparent aminosilicone oil microemulsion of the average particle size below 0.05 micron was prepared. The interaction of the aminosilicone oil, water, complex surfactants and cosurfactant was studied by part pseudoternary phase diagram. The effect of cosurfactants (such as alcohol) and the mechanism of its effect on the phase behaviour of the pseudoternary system were investigated.
Crystal Structures and Magnetic Properties of Two New Schiff Base Complexes
Guang Xiang LIU , Xiao Ming REN , Heng XU , Chuan Yi TANG , Gen Hua WU , You Cun CHEN
2004, 15(9): 1105-1108
[Abstract](187) [FullText HTML] [PDF 1689KB](0)
Two new Schiff base complexes,[NiL]ClO4 1 and [CuL]ClO4·0.5H2O 2, were synthesized and characterized, where L is the 1:1 condensation product of salicylaldehyde and diethylenetriamine. Their crystal structures and magnetic properties were determined and investigated. The H-bonding interactions concern just in neighbor cation and anion, do not extend into network for both 1 and 2. The temperature dependence of the magnetic susceptibilities (2-300K) showed that 1 is diamagnetism and 2 is paramagnetism with weak antiferromagnetic exchange interactions between adjacent spin carriers, no magnetic ordering taking place in these two complexes.
Synthesis and Characterization of Samarium (Ⅲ) Containing Poly-(N-vinylacetamide) Complex
Yan CAI , Ming Qing CHEN , Juan XU , Pin Fang WU , Akashi MITSURU , Xiao Hua HUANG
2004, 15(9): 1109-1112
[Abstract](185) [FullText HTML] [PDF 1334KB](0)
Poly (N-vinylacetamide) (PNVA) was synthesized by the free radical polymerization and its samarium (Ⅲ) binary complex was prepared and characterized by means of IR, UV-vis, X-ray photoelectron spectroscopy (XPS) and fluorescence spectra. The fluorescent intensity of samarium (Ⅲ) characteristic emission was increased significantly due to efficient energy transfer from polymeric ligand to Sm (Ⅲ) ion in the complex.
Photoelectrochemical Properties of Highly Oriented ZnO Nanotube Array Films on ITO Substrates
Min GUO , Peng DIAO , Sheng Min CAI
2004, 15(9): 1113-1116
[Abstract](190) [FullText HTML] [PDF 1759KB](0)
Highly oriented ZnO nanotube array films on the conducting substrates have been synthesized by a simple hydrothermal method and characterized by scanning electron microscopy (SEM) and UV-Vis spectroscopy. The thin films consisting of laterally fragmentized ZnO nanotubes with controlled orientation have been tested as photoanode in Gr?tzel-type solar cell. For a sandwich-type cell, with 0.5 mol/L LiI and 0.05 mol/L I2 in propylene carbonate electrolyte, the overall solar energy conversion efficiency reaches 2.3%.
A Selective Colorimetric Anion Sensor Based on Di (hydroxymethyl) Di-(2-pyrrolyl) methane-TCBQ System
Yong GUO , Shi Jun SHAO , Jian XU , Yan Pin SHI , Sheng Xiang JIANG
2004, 15(9): 1117-1119
[Abstract](193) [FullText HTML] [PDF 1167KB](0)
A new class of non-covalent charge-transfer complex for anion sensing, consisting of di(hydroxymethyl) di-(2-pyrrolyl) methane and chloranil (TCBQ) is characterized. The new colorimetric anion sensors can generate visual color change against PO43- and HPO42- anions in EtOH/H2O (1:1 v/v) mixture solution. The dipyrromethane-quinone aggregations may be used for higher selective detection of PO43- than other inorganic anions in water solution.
Enlarged Area A-type Zeolite Membranes Prepared by Vacuum Seeding Method
Ai Sheng HUANG , Jie LIU , Wei Shen YANG
2004, 15(9): 1120-1122
[Abstract](173) [FullText HTML] [PDF 1051KB](0)
High quality A-type zeolite membranes, with enlarged area over 70 cm2, were successfully synthesized on a tubular (-Al2O3 support by applying the vacuum seeding method.
Enhancing the Deactivation Durability of Nano-sized HZSM-5 for Aromatization by Adjusting its Ratio of Lewis/Brφnsted Acid Sites
Zhou Bo XU , Hong Chen GUO , Xiang Sheng WANG , Pei Qing ZHANG , Le Ping ZHAO , Yong Kang HU
2004, 15(9): 1123-1126
[Abstract](204) [FullText HTML] [PDF 1379KB](0)
Ratio of Lewis/Brφnsted acid sites (Cl/Cb) on the surface of nano-sized HZSM-5 was successfully manipulated by means of steaming and acid leaching. Significant enhancement of the deactivation durability of nano-sized HZSM-5 in the aromatization of fluid catalytic cracking (FCC) gasoline olefins seems to be closely related to the increase of Lewis/Brφnsted acid sites ratio.
Preparation of A New Fiber by Sol-gel Technology in Solid-phase Microextraction (SPME)
Li Ming WEI , Qing Yu OU , Ju Bai LI
2004, 15(9): 1127-1130
[Abstract](194) [FullText HTML] [PDF 1569KB](0)
The sol-gel technology is applied for the preparation of solid-phase microextraction (SPME) fiber. The fiber demonstrates high thermal stability, efficient extraction rate and the selectivity for non-polar or low-polar analytes. Efficient SPME-GC-FID analyses of benzene-toluene-ethylbenzene-xylenes (BTEXs) and low-polar halocarbon were achieved by the sol-gel coated DSDA-DDBT-TiO2 fiber. Some parameters of the SPME fiber for the determination of halocarbon in aqueous sample were investigated.
Room Temperature Phosphorescence pH Switch Based on Photo-induced Electron Transfer
Li Xuan MU , Yu WANG , Zhao ZHANG , Wei Jun JIN
2004, 15(9): 1131-1134
[Abstract](192) [FullText HTML] [PDF 1470KB](2)
In this paper, photoinduced electron transfer(PET) phosphoroionophore, N-(1-bromo-2-naphthylmethyl)-diethanolamine (BND) was synthesized and its phosphorescent characteristics were studied. The experimental results showed that strong phosphorescence could be observed in β-cyclodextrin aqueous solution only at low pH value. This system combined AND and NOT function to produce a three-input inhibit (INH) logic gate.
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