1998 Volume 9 Issue 11

Cyclization Reaction of α-Triazolyl-α, β-unsaturated Ketones with Phenyl hydrazine
Guo Feng ZHAO , Jun REN , Yu Chang LI , Gui Yu JIN
1998, 9(11): 979-982
[Abstract](180) [FullText HTML] [PDF 122KB](0)
The reaction of α-triazolyl-α, β-unsaturated ketones with phenyl hydrazine was studied. The result indicated that cyclization took place and new heterocyclic compounds of substituted 4,5-2H-pyrazoles were obtained, whose structures and conformation were characterized by 1H NMR, IR, MS, elemental analysis and X-ray diffraction.
N-Arylindne 1,4-Cycloaddition Reaction.Preparation of Substituted Hexahydrofurol [3,2-c] quinolines
Jun ZHAO , Shu Feng CHEN , Xiao Tian LIANG
1998, 9(11): 983-985
[Abstract](194) [FullText HTML] [PDF 97KB](0)
Lewis acid catalyzed cycloaddition reactions of N-arylideneaniline I with 2,3-dihydrofuran gave a pair of epimers dl-2, 3,3a, 4,5, 9b-hexahydro-4-arylfuro [3,2-c] quinolines and Ⅲ') and a few of their corresponding aromatized compounds .
Synthesis of an Anti-1,3-Diol Type Chiral Building Block
Yong Wu , Mei GUAN
1998, 9(11): 987-988
[Abstract](180) [FullText HTML] [PDF 58KB](0)
A chiral building block, anti-l,3-diol 2,has been synthesized in 7 steps, starting from readily available and inexpensive D-(+)-xylose.
Stable Send-ketals of 3',5'-O-(Tetraisopropyldisiloxane-1,3-diyl)-2'-Ketouridine
Guo Chen CHI , Zhong Biao ZHANG , Xiao Hua Xu , Ru Yu CHEN
1998, 9(11): 989-992
[Abstract](173) [FullText HTML] [PDF 105KB](0)
A series of stable semi-ketals were obtained via the reactions of 3',5'-0-(tetraisopropyldisiloxane-l, 3-diyl)-2'-ketouridine 1 with primary alcohols. In the addition reaction, only a single diastereomer was observed. The configuration of 3b was confirmed by X-ray diffraction.
A New Chromogenic Diester-calix [4]crown Receptor for Ca2+
Chuan Feng CHEN , Qi Yu ZHENG , Zhi Tang HUANG
1998, 9(11): 993-996
[Abstract](174) [FullText HTML] [PDF 117KB](0)
A diester-calix [4]crown-4-ether bearing mono (azophenol) moiety shows a larger spectral change toward Ca2+ than other alkali and alkaline earth cations.
Stereoselective Synthesis and Bioactivities of New ω-Azolyalkenes
Shui Ming LU , Wen Jing XIAO , Wen Fang HUANG , Tian Jie WU
1998, 9(11): 997-998
[Abstract](177) [FullText HTML] [PDF 65KB](0)
A series of new ω-azolylalkenes 3 were synthesized by N-alkylation of obromoalkenes 2 which were obtained by Witting reaction of o-hydroxyalkylphosphonium bromide with aromatic aldehydes and subsequent bromination. The structures of products were confirmed by 1HNMR, IR, MS and elemental analysis. The preliminary bioassay indicated that some of them had high fungicidal activities.
The Stereoselective Formal Synthesis of (-)-Slaframine
Han Qing DONG , Guo Qiang LIN
1998, 9(11): 999-1002
[Abstract](180) [FullText HTML] [PDF 147KB](0)
The stereoselective synthesis of (-)-slafrarninc has been achieved by utilizing the Sharplcss asymmetric epoxidation of divinylcarbinol (2) and the regio-selcctive dihydroxylation of compound 4 as the key steps.
Synthesis of the Natural Products Resveratrol (Ⅰ) and Isorhapotogenin (Ⅱ)
Ya Bing FENG , Lin WANG , Zhi Zhong ZHAO
1998, 9(11): 1003-1004
[Abstract](182) [FullText HTML] [PDF 78KB](0)
We have synthesized two natural products, resveratrol I and isorhapotigcnin Ⅱ by 8 and 7 step reaction sequence, respectively. The synthetic products I and Ⅱ were characterized by IR, MS, 1H-NMR in comparison with the corresponding natural products.
A Theoretical Research on the Intermediate in the Reaction of N-Phosphorylamino-acid to form Peptide or Ribotide
Ru Gang ZHONG , Zhao Long LI , Yu Fen ZHAO , Qian Huan DAI
1998, 9(11): 1005-1006
[Abstract](186) [FullText HTML] [PDF 79KB](0)
In order to explain the high activity of N-phosphoryl-α-amino acids, ab initio and MNDO calculations are performed to study the reaction pathway of the intermediate formation from N-dimethylphosphoryl-a-alanine (DMP-α-Ala) and the structures and energies involved in the reaction.
The oretical Study on the Pyrolysis Mechanism and Kinetics of 3-Hydroxy-3-Methyl-2-Butanone
Wen Lin FENG , Jie Hao CHEN , Yan WANG
1998, 9(11): 1007-1008
[Abstract](178) [FullText HTML] [PDF 77KB](0)
The mechanism and kinetics for the decomposition of 3-hydroxy-3-methyl-2-butanone have been studied by using the ab initio RHF/3-21G method. The calculated activation barrier of the reaction is 249.6kJ/mol which is in reasonable agreement with the experimental data (222.2±3kJ/mol). The calculated results show that the decomposition is a concerted process with hydrogen transferring and bond breaking via a five-membered cyclic transition state. The thermal rate constants of the decomposition are obtained by calculating microcanonical probability fluxes through transition state1.
Inner Sphere Reorganization Energy for the Electron Transfer Reactions between M-C6H6 and M+-C6H6 Complexes in Gaseous phase:An ab initio Computation
Zheng Yu ZHOU , Jian XU , Chuan Song ZHANG , Xing Ming ZHOU
1998, 9(11): 1009-1012
[Abstract](191) [FullText HTML] [PDF 156KB](0)
An ab initio computation of reorganization energy for the electron transfer reactions between metal atom-benzene and ion-benzene complexes is presented by using of both the George-Griffith-Marcus (GGM) method and Hessian matrix method. The results suggest that the coupling interactions between different vibrational modes are very important to caclculation the inner sphere reorganization energy for electron transfer reactions in gaseous phase.
A Pair of Dimeric Stilbene Epimers from Gnetum Montanum
Hao CHEN , Mao LIN
1998, 9(11): 1013-1015
[Abstract](186) [FullText HTML] [PDF 125KB](1)
A pair of dimeric stilbenes, gnetifolin M and gnetifolin N were isolated from the lianas of Gnetum montanum. All attempts to separate them by HPLC were unsuccessful. Their structures were elucidated by the spectroscopic analysis including 2D-NMR studies on the peracetate.
Two New Taxoids from Taxus Yunnanensis
Sheng Hong LI , Hong Jie ZHANG , Ping YAO , Han Dong SUN
1998, 9(11): 1017-1020
[Abstract](177) [FullText HTML] [PDF 150KB](0)
Two new baccatin Ⅲ type taxoids, 13-Cinnamoylbaccatin Ⅲ (1) and 7-xylosylbaccatin Ⅲ (2), have been isolated from the barks of Taxus yunnanensis. The structures were elucidated by spectral means.
Four New Diterpenoids from Isodon leucophylla
Shao Nong CHEN , Shao Yuan CHEN , Zhong Wen LIN , Fang Di NIUBo Gong LI , Han Dong SUN , Yao Zu CHEN
1998, 9(11): 1021-1024
[Abstract](169) [FullText HTML] [PDF 195KB](0)
Four new diterpenoids, baiyecrystals A-C and epi-baiyecrystal C,were isolated from I. leucophylla. Their structures were determined by means of spectral methods as 1-4.
Three New Diterpenoids from Isodon Eriocalyx
Shao Nong CHEN , Shao Yuan CHEN , Jian Min YUE , Zhong Wen LINGuo Wei QIN , Han Dong SUN , Yao Zu CHEN
1998, 9(11): 1025-1028
[Abstract](183) [FullText HTML] [PDF 143KB](0)
Three new diterpenoids, eriocalyxins C-E, were isolated from Isodon eriocalyx. Their structures were elucidated as 6β-hydroxy-15β-acetoxy-3α, 20-epoxy-16β, 17-epoxy-ent-kaur-1, 7-dione; la, 7β-dihydroxy-6β, 15β-diacetoxy-7, 20-epoxy-ent-kaur-16-ene; and 15β-acetoxy-l, 6-dioxo-6, 7-seco-ent-kaur-2, 16-dien-7, 20-olide by means of spectroscopic methods, including two-dimensional NMR techniques.
New Alkaloids from the Rhizomes of Goniothalamus Griffithii
Yan Jun ZHANG , Man KONG , Ruo Yun CHEN , De Quan YU
1998, 9(11): 1029-1032
[Abstract](177) [FullText HTML] [PDF 153KB](0)
Three new alkaloids, griffithclionc 1,griffiazanonc A 2 and griffiazanone B 3 were isolated from the rhizomes of Goniothalcimus griffithii Hook. F. et. Thorns. Their structures were elucidated by analysis the spectral data (IR, UV, MS, 1H and 13C NMR, HMBC, NOE experiment). The absolute configuration of griffithazanonc A 2 was determined by Mosher's methods.
Stability and Luminescence Properties of Tb (Ⅲ) Complexes with Adrenaline
Feng GAO , Jing Fen HAN , Zhi Jian WU , Shu Yun WANGChun Ji NIU , Jia Zuan NI
1998, 9(11): 1033-1034
[Abstract](182) [FullText HTML] [PDF 88KB](0)
Stability and luminescence properties of Tb (Ⅲ) complexes with adrenaline have been studied. The Tb (Ⅲ) complexes with adrenaline are quite stable. The fluorescence spectra of the Tb (Ⅲ) complexes with adrenaline show the characteristic fluorescence bands of Tb (Ⅲ) ions which are attributed to energy transfer from ligands to Tb (Ⅲ) ions.
Liposome Immunoassay for Determination of Phenytoin
Wen Yu ZHU , Wen Bao CHANG , Yun Xiang CI
1998, 9(11): 1035-1038
[Abstract](175) [FullText HTML] [PDF 150KB](0)
Homogeneous liposome immunoassay for the determination of phenytoin was studied. Liposomes were prepared from cholesterol (CH) and phospholipids including dipalmitoyl phosphatidyl ethanolamine (DPPE) for conjugation with thiol-containing antibodies. Hemin chloride was entrapped in the liposome and antibody was modified by reaction with 3-(2-pyridyl-dithio) propionyl N-hydroxysuccinimidc ester (SPDP) to introduce thiol groups for efficient coupling. Antibody-coupled liposomes (immunoliposomes) were incubated with phenytoin and complement, and then with hemin substrate. The amount of hemin released from immunoliposomes, which increases with concentration increase of phenytoin, can be detected rapidly by determining the fluorescence with its substrate p-hydroxyphenyl propionic acid (HPPA) and hydrogen peroxide.
The Amperometric Glucose Enzyme Electrode by Immobilized Glucose Oxidase in Glucose oxidase/N-ethyl-Poly (4-vinyl)pyridine Multilayer
Yuan Zhong MA
1998, 9(11): 1039-1041
[Abstract](191) [FullText HTML] [PDF 126KB](0)
Multilayers of glucose oxidase (GOD)/N-ethyl-poly (4-vinyl) pyridine (EPVP) have been assembled on thiol self-assembled monolayers on gold electrode. Tliis electrode can be used as an amperometric enzyme electrode for glucosc. Fe (CN)63_/4_ incorporated in EPVP layer acts as the electron mediator, the linear range was 0.1 to 6mmol/L when the number of GOD layers was 5.
Separation of Hydrophobic Neutral Compounds by Microemulsion Electrokinetic Chromatography
Xiao Yun FU , Xiu Zhu XU , Jian De LU
1998, 9(11): 1043-1044
[Abstract](170) [FullText HTML] [PDF 87KB](2)
Microemulsion electrokinetic chromatography (MEEKC) was developed for the separation of hydrophobic neutral compounds. The effects of core phase and co-surfactant on the separations were investigated. Under the selected condition, good resolutions were obtained for the test mixtures. The separation efficiencies were higher than 105 theoretical plates per metre.
Synthesis of Monodisperse Poly (chloromethylstyrene divinylbenzene) Particle and Its Applications
Yin Mao WEI , Xin Du GENG
1998, 9(11): 1045-1048
[Abstract](172) [FullText HTML] [PDF 495KB](0)
Monodisperse poly (chloromethylstyrene divinylbenzene) particles were prepared by a two-step swelling method. It was demonstrated that the packings have comparative advantages for biopolymer separation with high column efficiency, low interstitial volume and low back pressure to the packings prepared with suspension polymerization method. Using size exclusion chromatography and weak ion exchange chromatography as examples, it was shown that these packings could be modified chemically more easily than poly (styrene divinylbenzene) packings.
Relationship between the Conformation and Enzyme Activity of Commercial and Purified Glucose Oxidase
Guo Liang DAI , Jin Ru LI , Long JIANG
1998, 9(11): 1049-1050
[Abstract](183) [FullText HTML] [PDF 85KB](0)
Relationship between the conformation and enzyme activity of the commercial and purified GOD have been studied. Both enzyme activity and value of α/β of purified GOD in water solution and LB film were higher than that of commercial GOD.
Inclusion Complexation of β-CD with Phenothiazine and N-Alkylphenothiazine Derivatives
Wen Guang LI , Xiu Qin RUAN , Qing Xiang GUO , You Cheng LIU
1998, 9(11): 1051-1054
[Abstract](172) [FullText HTML] [PDF 118KB](0)
Inclusion of β-cyclodextrin (β-CD) with phenothiazine 1 and N-alkylpheno-thiazine derivatives (alkyl=ethyl 2, isobutyl 3 and isopentyl 4) in aqueous solution was studied by means of UV-vis spectroscopy. The association constant Ka values for the inclusion of β-CD with 1,2, 3 and 4 were determined to be 188, 214, 129 and 80 L/mol, respectively. It indicates that the stability of the inclusion complexes is dependent on the structure and the volume of the substituents in the guest compounds.
Preparation of Amorphous Film on Ni-S Alloy by Electroplating Method
Min DU , Rong Jie GAO , Xu Jun WEI
1998, 9(11): 1055-1058
[Abstract](170) [FullText HTML] [PDF 126KB](0)
Beginning from the formation of amorphous alloy film and its use of promise, this paper obtains the Ni-S amorphous alloy film by electroplating method using a bath containing Na2S2O3, and considers the deposition conditions in detail. The composition of Ni-S alloy film changes with the cathodic current density, Na2S2O3 content in the bath solution and bath pH, but the structure of the film is determined by the sulphur content in the deposit. X-ray diffraction (XRD) patterns show that films containing about 15-30% sulphur consist of amorphous alloy. In addition, the process of Ni-S alloy film deposition and the relation between the plating conditions and deposits were studied.
Novel Vesicular Aqueous Two-Phase Systems
Guo Xi ZHAO , Wang Lin YU , Yu Jun GONG , Bu Yao ZHU
1998, 9(11): 1059-1062
[Abstract](169) [FullText HTML] [PDF 631KB](1)
The interesting phenopmena of two aqueous phases coexisting in dilute aqueous solutions of sodium undecenoate-dodecyltrimethylammonium bromide mixture and sodium laurate-dodecyltrimethylammonium bromide mixture were investigated. Vesicles existing in both phases were shown by TEM images. The vesicles are dispersed in lower phase and flocculated in upper phase. Multilamellar structure of vesicles was found in the upper phase of sodium laurate-dodecyltrimethylammonium bromide system.
Study on the Bond Covalency and Bond Susceptibility in NdCr1-xMxO3 (M=Mn, Fe, Co)
Zhi Jian WU , Qing Bo MENG , Si Yuan ZHANG
1998, 9(11): 1063-1066
[Abstract](175) [FullText HTML] [PDF 171KB](0)
Bond covalency, bond susceptibility and macroscopic linear susceptibility in NdCr1-x. xMxO3 (M=Mn, Fe, Co, 0.0 ≤ x ≤ 1.0) are investigated by complex chemical bond theory. The results indicate the bond covalencies are insensitive to the doping level. With the increasing doping level, the macroscopic linear susceptibilities increase for M=Mn, Fe, decrease for M=Co. The valence state of Cr can be strongly influenced by the properties of the doping ions.
Synthesis and Crystal Structure of Complex of Sodium Perrhenate with Tetraethyl p-tert-Butylcalix [4] arene Tetraacetate
Zhi Xian ZHOU , Yan Jun XING , Kui LU , Yang Jie WU
1998, 9(11): 1067-1068
[Abstract](180) [FullText HTML] [PDF 78KB](0)
The complex of sodium perrhenate with ester derivative of calix [4] arene having the stoichiometric formula [NaL]ReO4·H20, was prepared. The X-ray structure analysis revealed that the sodium ion is coordinated to four ether and four carbonyl oxygen atoms giving a coordination number of eight with a tetragonal antiprism configuration. The complex cation [NaL]+ and anion ReO4- are linked by electrostatic attraction.
Synthesis and Crystul Structure of A New Mixed-Valence Complex of Copper (Ⅰ, Ⅱ) α-Methacrylate with Triphenylphosphine and Methanol
Yao Yu WANG , Qian SHI , Qi Zhen SHI , Yi Ci GAO , Zhong Yuan ZHOU
1998, 9(11): 1069-1072
[Abstract](169) [FullText HTML] [PDF 137KB](0)
Copper (Ⅱ) α-methacrylate reacts with triphenylphosphine to form mixed-valence copper (Ⅰ,Ⅱ) complex Cu4 (CH2=C(CH3)COO)6 (PPh3)4 (CH3OH)2 in methanol solution. The crystal and molecular structure of the complex has been determined by single crystal X-ray structural analysis. This material forms pale green crystals with triclinic symmetry, space group Pi, a=1.3567(2) nm, b=1.3946(3)nm, c=1.4569(3)nm, α=66.069(14)°,β=84.234(14)°, γ=69.975 (13)°, R=0.0536.
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