1997 Volume 8 Issue 3

Reaction of Phenylethyne with 2,4-Pentanedione in the Presence of Manganese(Ⅲ) Acetate and Oxygen
Chang YI QIAN , Bo HAN , Yu Fen ZHAO , Yoshikazu NOIRI , Hiroshi NISHINO , Kazu KUROSAWA
1997, 8(3): 189-190
[Abstract](280) [FullText HTML] [PDF 93KB](1)
The reaction of phenylethyne with 2,4-pentanedione in the presence of manganese(Ⅲ) acetate and oxygen at room temprature gave 4-acetyl-5-benzoyl-3-methyl-1,2-dioxolan-3-ol, 2-acetyl-3-benzoloxirane and 3-acetyl-2-methyl-phenylfuran.
Novel Reduction of Sodium Alkyl Thiosulfates to Disulfides with TiCl4/Sm System
Hong Yun GUO , You HUANG , Yong Min ZHANG
1997, 8(3): 191-192
[Abstract](189) [FullText HTML] [PDF 76KB](0)
Sodium alkyl thiosulfates(Bunte salts) can be readily reduced to the corresponding disulfides with TiCl4/Sm system in good to excellent yields under mild conditions.
Nucleophilic Aromatic Substitution of Nitrobenzenes with Nitrite Ion
Zhi Qiang ZHANG , Zheng Hua TIAN
1997, 8(3): 193-194
[Abstract](183) [FullText HTML] [PDF 89KB](0)
It is experimentally found that different reaction courses exist when nitrite ion reacts with nitrobenzenes with different electron withdrawing groups.When it is substituted with strong electron withdrawing groups.self-condensation in aprotic polar solvent occurs to give symmetrical disubstituted diphenyl ethers.However.when it is substituted with moderate electron withdrawing groups,no diphenyl ethers are obtained under the same conditions,instead,corresponding carboxylates are yielded.As a result,the applicability of this reaction is distinctly clarified.
Syntheses of (3-Benzyl-4-Aroyl-1,2,4-Triazole-5-yl)[5-(3,4,5-Trimethoxylphenyl)-1,3,4-Oxadizole-2-yl] Sulfides
Xiao Ming FENG , Rong CHEN , Lian Fu TANG , Yao Zhong JIANG
1997, 8(3): 195-198
[Abstract](182) [FullText HTML] [PDF 137KB](0)
Twelve new (3-benzyl-4-aroyl-1,2,4-triazole-5-yl)[5-(3,4,5-trimethoxyphenyl)-1,3,4-oxadiazole-2-yl] sulfides(2) have been synthesized from the nucieophilic displacements of 3-benzyl-4-aroyl-1,2,4-triazole-5-hydrosulfuryl anion on the 2-position of 2-methylsulfonyl-5-(3,4,5-trimethoxyphenyl)-1,3,4-oxadiazole(1).Compounds(2) were screened for their antibacterial activity against E.Coli at 0.01%.The results show that some compounds(2) have strong inhibiting effects.
Synthesis and Diastereomeric Analysis of Uridine 2',3'-Cyclic Phosphite
Yun DING , Yi Bing ZHANG , Yao Quan CHEN
1997, 8(3): 199-202
[Abstract](178) [FullText HTML] [PDF 150KB](0)
Uridine 2',3'-cyclic phosphite has been synthesized and the diastereomers were analysed by 2D NMR technique to assign the configuration.
Studies on the Total Synthesis of Hainanolide (Ⅲ)-Unusual Diene Isomerization in a Diels-Alder Reaction
Wen Qian YANG , Lu Yan ZHANG , Shi Zhi CHEN , Liang HUANG
1997, 8(3): 203-204
[Abstract](184) [FullText HTML] [PDF 96KB](0)
An unexpected diene isomerization of the triene acid 3 in the Lewis acid catalyzed intramolecular Diels-Alder reaction was observed.
Total Synthesis of Przewaquinone A
Wen Hu DUAN , Jun Chao CAI
1997, 8(3): 205-206
[Abstract](274) [FullText HTML] [PDF 60KB](0)
Przewaquinone A, a natural orthoquinone was synthesized through several steps,the analytic data of the synthetic target compound was identical with that of przewaquinone A.
Synthesis of New Spin Labeled Derivatives of Podophyllotoxin as Potential Anticancer Agents
Jian Lin PAN , Yan Guang WANG , Jian Feng SHI , Yao Zu CHEN
1997, 8(3): 207-208
[Abstract](181) [FullText HTML] [PDF 99KB](0)
Five new nitroxyl spin labeled podophyllotoxins (2-6) have been synthesized. Compounds 2 and 3 have been tested for their anticancer activity in vitro.The results showed that compound 3 is much more potent than the clinically used etoposide (VP-16) in its inhibition of P388 cells,while compound 2 is not active.
Synthesis of Bis(macrocyclic) Polyamines Containing Rigid Bridging Groups
Hong Jun WANG , Cheng Tai WU
1997, 8(3): 209-212
[Abstract](187) [FullText HTML] [PDF 142KB](0)
This paper deals with the synthesis of three new symmetrical bis (macrocylic) polyamines and their dinuclear copper (Ⅱ) complexes.All these compounds were identified by elemental analysis and spectral analysis (IR,1H and 13C NMR).
Calixthiacrown:A New Multidentate Ligand for Platinum Metal
Yuan Yin CHEN , Zhen Lin ZHONG , Yi Sui ZHOU , Bao Lian ZHANG , Xue Ran LU
1997, 8(3): 213-214
[Abstract](181) [FullText HTML] [PDF 94KB](0)
5,11,17,23-Tetra-tertbutyl-25,27-dihydroxy-26,28-1',7',13'-trioxa-4',10'-dithiatridecene calix[4]arene (Calix[4]dithiacrown-5) was synthesized from tetra-tert-butyl-calix[4]arene via 1,3-lower rim functionallization with chloroethyltosylate,followed by ring-closing condensation with β,β'-dimercaptoethyl ether in the presence of sodium ethoxide as a base under nitrogen atmosphere.It was found that the calix[4]dithiacrown-5 can form a platinum complex and the complex can catalyze the hydrosilylation of olefins with triethoxysilane efficiently.
Synthesis of Methylated β-Cyclodextrins Derived Optically Active Poly(N-diphenylmethyl maleimide)
Wei Hong LIU , Yong Ming CHEN , Chuan Fu CHEN , Fu XI
1997, 8(3): 215-218
[Abstract](173) [FullText HTML] [PDF 175KB](0)
The methylated β-cyclodextrins derived optically active polymers are first synthesized through asymmetric polymerization of N-diphenylmethyl maleimide with lithium salt of heptakis (2,6-O-dimethyl) β-cyclodextrin (DM-β-CD) as an initiator.The resulting polymers show negative specific rotation which is opposite in sign to that of DM-β-CD.The asymmetric induction is further confirmed by circular dichroism.The structure is characterized by IR and NMR spectroscopies.
Strong Inclusion Complexation Using Hydroxypropyl-β-Cyclodextrin as Host Molecule
Shu Qin LIU , Hui Zhi FAN , Wen Hui JIA , Jing Hao PAN
1997, 8(3): 219-220
[Abstract](186) [FullText HTML] [PDF 75KB](0)
Inclusion complexes of nitro-compounds using β-cyclodextrin and hydroxypropyl-β-cyclodextrin as host molecule have been studied by cyclic voltammetric method.The inclusion constants of the corresponding complexes have been determined.Strong inclusion complexation by hydroxypropyl-β-cyclodextrin has been verified.
Photochemical Reaction of 9,10-Anthraquinone Labeled Bovine Serum Albumin Conjugate
Qing Zhi ZHU , Jin Gou XU , Xiang Qun GUO , Xue Ying ZHENG , Wen You LI , Yi Bing ZHAO
1997, 8(3): 221-224
[Abstract](180) [FullText HTML] [PDF 186KB](0)
Bovine serum albumin (BSA) was labeled with 9,10-anthraquinone and the photochemical fluorimetric reactivity of the covalently conjugated 9,10-anthraquinone was remarkably improved.The mechanism for the enhancement in the photochemical reactivity of conjugated 9,10-anthraquinone with BSA was discussed.
A New Caffeoyl Conjugate from Erigeron Breviscapus
Jian Min YUE , Zhong Wen LIN , Han Dong SUN
1997, 8(3): 225-228
[Abstract](183) [FullText HTML] [PDF 184KB](0)
Erigoster A (1a),a new compound with a novel basic skeleton,was isolated from Erigeron breviscapus.The structure elucidation and complete proton and carbon NMR assignments were achieved by the utilization of a combination of two-dimensional NMR techniques.
Daphkoreanin,a New Coumarin Glucoside from Daphne Koreana
Yan Ze LIU , Gang DING , Chun Ru JI , Yang Jie WU
1997, 8(3): 229-230
[Abstract](193) [FullText HTML] [PDF 75KB](0)
A new coumarin glucoside,daphkoreanin,has been isolated from the roots and stems of Daphne koreana.Its structure was established as 5-methoxy-7-hydroxy coumarin-8-O-β-D-glucoside by physico-chemical properties and 1HNMR spectral analysis.
Taxuchin B, a New Chlorine-Containing Taxoid
Wei Shuo FANG , Qi Cheng FANG , Xiao Tian LIANG , Yang LU , Nan WU , Qi Tai ZHENG
1997, 8(3): 231-232
[Abstract](186) [FullText HTML] [PDF 121KB](0)
A new taxoid,taxuchin B[1],has been isolated from twigs and needles of Taxus chinensis.It is the first chlorine-containing taxoid reported to date.
Donhexocin, a New Non-tetrahydrofuran Acetogenin from Goniothalamus Donnaiensis
Zhong JIANG , De Quan YU
1997, 8(3): 233-234
[Abstract](192) [FullText HTML] [PDF 86KB](0)
A novel bioactive Amionaceous acetogenin,donhexocin (1),has been isolated from the roots of Goniothalamus donnaiensis (Annonaceae).1 is a new acetogenin lacking THF rings but bearing six hydroxyls including two vic-diol systems in the aliphatic chain.Its structure and stereochemistry has been elucidated by spectoscopic analysis and derivatization.
A New Cytotoxic Dihydroxy Sterol from Laurencia Majuscula
Xiao Hua XU , Jing Yu SU
1997, 8(3): 235-236
[Abstract](189) [FullText HTML] [PDF 82KB](1)
24s-Stigmasta,4,25-diene,3β,6β-diol 1,a new sterol has been isolated from the algae Laurencia majuscula collected from the south China sea.Its structure was elucidated by spectroscopic methods.Compound 1 was cytotoxic against the P-388 cell line with an IC50 value of 1.2 μg/ml.
Alkaloids from Isatis indigotica
Ke Min DENG , Xiao Yun WU , Gen Jin YANG , Guo Wei QIN
1997, 8(3): 237-238
[Abstract](182) [FullText HTML] [PDF 105KB](0)
Isaindigotone 1 and 3-(2'-hydroxyphenyl)-4(3H)-quinazolinone 2 were isolated from the roots of Isatis indigotica.Compound 1 was elucidated as a new alkaloid.Compound 2 was discovered for the first time from a natural source.
Spectroscopic Properties of a Novel Zinc Phthalocyanine with four 17-Membered Crown Ether Voids
Guo Xiang XIONG , Jian Ping YE , Hui Jun XU
1997, 8(3): 239-242
[Abstract](178) [FullText HTML] [PDF 142KB](0)
A zinc phthalocyanine containing (17-crown-5) ether subunits has been synthesized.UV-visible absorption and fluorescence emission spectra and associated photophysical parameters have been determined.In addition to the fluorescence at 710 nm from S1.a strong upper excited state emission around 424 nm has been detected.X-ray structural analysis showed that the crown ether unit is conformationally deformed and oblate like that accounted for the unusual spectroscopic properties.
Studies on Synthesis of Stationary Phase Containing Nicotinamide Adenine Dinucleotide (NAD) Bonded to Phospholipid-Coated Aminated Silica for HPLC
Jin Mao YOU , Zong Qin RUAN , Jing Wu KANG
1997, 8(3): 243-246
[Abstract](181) [FullText HTML] [PDF 205KB](0)
Recently biospecific affinity chromatography has been widely used for the separation and purification of various enzymes and nucleic acids.In this paper,a series of synthetic reactions of solid-liquid phase were carried out on silica surface,using a macroporous (30μm), microspherical silica (8μm) as the matrix and γ-aminopropyltriethoxysilane as the activating agent,the nicotinamide adenine dinucleotide (NAD) was bonded through its amino groups to the carboxylic groups of linked phospholipid which was bonded covalently on aminated support.The bonded stationary phase has high thermal stability,and could be used to separate of nucleotides with good resolution.
Studies on Zeolite Modified Electrode(Ⅰ)-Ascorbic Acid Sensor Based on Carbon Paste Electrode Containing Fe(Ⅲ) Y Zeolite
Ming Zhu ZOU , Hong Ding XU , Jie LU , Qin Hua Ru
1997, 8(3): 247-250
[Abstract](182) [FullText HTML] [PDF 176KB](0)
A new ascorbic acid sensor constituted of carbon paste and Fe(Ⅲ)Y zeolite was studied.The characters of the sensor such as linear range、potential window、apparent Michaelis constant、response time、stability and accuracy were investigated.The experimental results indicate that the analytical performance of the sensor is satisfactory.
A Neutral Carrier Based Phosphate Sensor with Anti-Hofmeister Behavior
Dong LIU , Wen Can CHEN , Rong Hua YANG , Ru Qin YU
1997, 8(3): 251-254
[Abstract](181) [FullText HTML] [PDF 162KB](0)
A PVC membrane electrode,using bis(tribenzyltin) oxide as the carrier,displayed selective response to hydrogen phosphate in the 5×10-6mol/L to 10-1mol/L activity range with a slope of -30.1mV/dec.in solutions of pH 7.2.The comparison of potential response characteristics between the binuclear and mononuclear organotin compounds has been made,showing that binuclear organometallic compounds may become a promising class of carriers for anions.
A New Catalyst for Hydrogen Transfer Hydrogenation of Acetophenone
Pian Pian XU , Rong Hui ZHENG , Jing Xing GAO , Pei Qing HUANG , Hui Lin WAN
1997, 8(3): 255-258
[Abstract](187) [FullText HTML] [PDF 166KB](0)
A new C2-symmetric diamine/diphosphine Ruthenium (Ⅱ) complex,RuCl2P2N2H4.was used as an excellent catalyst to carry out the catalytic hydrogen transfer reduction of acetophenone.The conversion of acetophenone to 2-phenylethanol was up to 99% under the following reaction conditions: substrate: Ru: (CH3)2CHOK=200:1:12; reaction temperature of 65℃,reaction time of 2 h.normal pressure.A hydride transfer mechanism was also discussed.
Synthesis and Crystal Structure of [Pd(NH3)4]Cl2·2[Pd(NH3)3Cl]Cl
Pei Feng XING , Peng Ji ZHAO , Rui Liang HUANG , Ze Ning HUANG , Xue An CHEN , Hong LIANG , Zhi Guang QIAN
1997, 8(3): 259-262
[Abstract](198) [FullText HTML] [PDF 165KB](0)
A new type of ammine palladium(Ⅱ) chloride was prepared by evaporating the solution of [Pd(NH3)]4Cl2 at room temperature.Its crystal structure was refined from single-crystal X-ray data:P42/nmc,a=10.5390(10)Å,c=16.905(3)Å,Z=2,and R=0.0357 for 731 structure factors and 52 variable parameters.The framework of the title compound is composed of three sorts of structural units: [Pd(NH3)4]2+, [Pd(NH3)3Cl]+,and Cl-,of which the first kind of least squares plane exhibits distortion in some degree.
Research on PbS Nanoparticles Coated with 2,6-O-Diallyl-β-CD
Yun LING , Lin GUO , Liang ZHANG , Xi Cheng AI , Ruo Nong FU , Qian Shu LI , He Sun ZHU
1997, 8(3): 263-266
[Abstract](198) [FullText HTML] [PDF 495KB](0)
PbS nanoparticles coated with 2,6-O-diallyl-β-CD were prepared successfully and characterized by transmission electron microscope (TEM),X-ray photoelectron spectrometer (XPS).The sample shows a very rapid induced absorption.
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