2003 Volume 14 Issue 1

Study on the Total Synthesis of Ecteinascidin 743 and Its Analogues──Construction of A Pentacyclic Intermediate
Ye Feng TANG , Zhan Zhu LIU , Shi Zhi CHEN
2003, 14(1): 1-2
[Abstract](627) [FullText HTML] [PDF 652KB](2)
Abstract:
A concise and efficient synthesis of the pentacyclic intermcdiate 1, as a simple model compound of Ectcinascidin 743 and its analogues, is described.
A Facile Synthesis of α-Phenylthio-α, β-Unsatuated Esters
Gui Sheng DENG , Zhi Zhen HUANG , Xian HUANG
2003, 14(1): 3-5
[Abstract](483) [FullText HTML] [PDF 952KB](1)
Abstract:
α-Phenylthio-α, β-unsaturated esters 6 were synthesized by Witting reaction of 3, which were prepared by a phenylsulfenyllation-trans-ylidation reaction.
Solid-Phase Total Synthesis of 1-β-Methylcarbapenem
Ming LEI , Cheng MA , Yan Guang WANG
2003, 14(1): 6-8
[Abstract](480) [FullText HTML] [PDF 829KB](6)
Abstract:
A 1-β-methylcarbapencm analogue 6 was synthcsized on polystyrene-dicthylsilane resin (PS-DES) using 2-azetidinone bearing with 2-oxazolidonc chiral auxiliary as starting matcrial.
Synthesis of A Novel Bridged Bis(β-cyclodextrin)s Possessing Phenan-throline Tether and Its Molecular Binding Ability with Dyes
Li LI , Peng LIANG , Yu LIU
2003, 14(1): 9-12
[Abstract](508) [FullText HTML] [PDF 1165KB](0)
Abstract:
A novel β-cyclodextrin dimer bearing 2, 9-diformyl-1, 10-phenanthroline tether 4 has been synthesized and its inclusion complexation behavior with two triangular model substrates(RhB and BG) has been investigated through fluorcseence and ultraviolet spectrometry. The result obtained indicated that novel bridged bis(β-cyclodcxtrin)s could significantly enhance the original molecular binding ability of native β-cyclodextrin by coopcrative binding of two hydrophobie cavities.
An Efficient Palladiun-catalyzed Coupling Reaction for the Preparation of Biaryls and Polyaryls
Zhi Yong WANG , Zheng Gen ZHA , Jia Hai ZHANG , Ji Hui WU
2003, 14(1): 13-16
[Abstract](481) [FullText HTML] [PDF 1320KB](3)
Abstract:
In the case of Pd(PPh3)4 as catalyst and toluene as reaction solvent, the desired biaryls and polyaryls were synthesized in excellent yicld and on a large scale.
A Novel Method for the Synthesis of Carboxylic Esters Catalyzed by Expandable Graphite
Ying Qun ZHANG , Chun WANG , Gui Shen LI
2003, 14(1): 17-19
[Abstract](500) [FullText HTML] [PDF 800KB](2)
Abstract:
Esterification reaction of carboxylic acid and alcohol has been carried out in excellent yield with expandable graphite as a catalyst.
Nano CaCO3:An Unique Condensation Agent for the Preparation of Monosubstituted Calix[4]arene by Ring-opening Reaction
Shu Ling GONG , Wei WANG , Peng Fei FANG , Yuan Yin CHEN
2003, 14(1): 20-21
[Abstract](465) [FullText HTML] [PDF 753KB](1)
Abstract:
Nano CaCO3 was used as a condensation agent in the ring-opening reaction of p-tert-butylcalix[4]arcnc with cpichlorohydrin to afford 5,11,17,23-tetra-tert-butyl-26,27,28-trihyd-roxy-25-(l'-chloro-2'-hydroxy-3'-propyl)calix[4]arcnc rcgiosclcctivcly in 52% yield. The yield was less lhan 2% by using normal CaCO3 instead of nano one under the same condilions.
Novel Water Soluble Fluorescent Trimethine Indocyanines Containing N-p-Carboxybenzyl Group
Li Qiu WANG , Xiao Jun PENG , Rong ZHANG , Guo Quan XU , Jing Nan CUI
2003, 14(1): 22-24
[Abstract](474) [FullText HTML] [PDF 998KB](0)
Abstract:
Two fluorescent indocyanine dyes containing at least one p-carboxybenzyl group on the nitrogen atoms in the hetcrocyclic rings were designed and synthesized. Their absorption maxima were 549 nm and 551 nm in water respectively. They had good water solubility and photostability.
An Efficient Synthesis of Aromatic 1-Hydroxymethylene-1,1-bisphosphonates from Aldehydes
Yu Li XIE , Qin ZHU , Xing Rong QIN , Yu Yuan XIE
2003, 14(1): 25-28
[Abstract](475) [FullText HTML] [PDF 1296KB](0)
Abstract:
A simple and efficient procedure for synthesis of 1-hydroxymcthylene-1,1-bisphosphoates from aldehydes is deseribed. This method was applied to the synthesis of nowel catcchol substituted bisphosphonatcs as the anti-ostcoporosis agents.
An Improved Synthesis of Retinoic Acid from β-Ionone
Yao Dong HUANG , Xiao Jie ZHANG , Ze Xu WANG , Fen Er CHEN
2003, 14(1): 29-31
[Abstract](460) [FullText HTML] [PDF 958KB](4)
Abstract:
A convenient and large-scale preparation of rctinoic acid 1 from β-ionone in five steps with 38% overall yield is described. The key steps are the epoxidization of 2 with a new methylated agent and the condensation 4 with tetraethyl methylenediphophonate in one-pot procedure to prepare 6.
Microwave-assisted Polymerization of ε-Caprolactone with Maleic Acid as Initiator and Drug Release Behavior of Ibuprofen-Poly(ε-caprolaetone) System
Ying SONG , Li Jian LIU , Ren Xi ZHUO
2003, 14(1): 32-34
[Abstract](510) [FullText HTML] [PDF 976KB](3)
Abstract:
Poly(ε-caprolactone) (PCL) with weight-average molar mass over 10000 g/mol was synthesized by microwave-assisted ring-opening polymerization of ε-caprolactonc (ε-CL) with malcic acid (MA) as initiator (2.45 GHz, 360 W, 85 min). Ibuprofen-PCL controlled release system was prepared directly by the ROP of ε-CL in its mixture with ibuprofen. The release of ibuprofen from the system was sustained and steady.
Synthesis and Characterization of Ferrocene-terminated Ruthenium Phenylacetylide Complexes with Alligator Clips
Heng Wei LIN , Xian Hong WANG , Xiao Jiang ZHAO , Ji LI , Fo Song WANG
2003, 14(1): 35-38
[Abstract](487) [FullText HTML] [PDF 1230KB](0)
Abstract:
Ferrocene-terminated trans-Ru(dppm)2 (dppm=Ph2PCH2PPh2)-containing molecular wires with alligator clips were prepared. They are suitable for self-asscmbly on gold electrode to investigate the influence of metal incorporation on the electron transportation property of the molecular wires.
Studies on Micellization of a Polystyrene-b-poly(acrylic acid) Copolymer in Aqueous Media by Pyrene Fluorescence
Zhi Huai SI , Guo Chang WANG , He Xian LI , Jia Long YUAN , Bing Lin HE
2003, 14(1): 39-42
[Abstract](503) [FullText HTML] [PDF 1646KB](1)
Abstract:
Pyrcnc probc and TEM have been employed to investigate the behavior of a polystyrenc-b-poly(acrylic aeid) (PS-b-PAA) copolymer in aqueous solution. A significant annealing temperature effect on the I1/I3 ratio of pyrene was observed and was interpreted in terms ofthe morphological change ofmicellar cores. Anncaling at a temperature higher than the glass transition temperature (Tg) of PS leads to densification ofthe hydrophobic core.
Synthesis and Photoluminescence of New Europium Complex Eu(DBM)3(DPPZ) with Dipyridophenazine Ligand
Bo LIANG , Mei Xiang ZHU , Wei Guo ZHU
2003, 14(1): 43-46
[Abstract](505) [FullText HTML] [PDF 1615KB](5)
Abstract:
Dipyrido [3, 2-a:2',3'-c] phenazine moiety has been introduced as neutral ligand in europium complex. Therefore, a new europium complex with saturated emission, strong fluorescent intensity and good solubility was designed and synthesized for the first time. Its photoluminescence and UV properties were examined. The experimental results showed that this new Eu-complex could be used as red electroluminescent materials.
Preparation of End Grafted Polyacrylonitrile Brushes through Surface Confined Radical Chain Transfer Reaction
Feng ZHOU , Shu Juan LIU , Bo WANG , Ting Mei WANG , Miao CHEN , Wei Min LIU
2003, 14(1): 47-50
[Abstract](497) [FullText HTML] [PDF 1099KB](2)
Abstract:
End grafted polyacrylonitrile (PAN) brush was prepared through surface initiated polymerization via the chain transfer process. The thiol-terminated monolayer and PAN brushes were characterized by FTIR, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), ellipsometry and contact angle measurements ete. It is demonstrated that radical chain transfer reaction and surface initiated precipitate polymerization can be used to prepare end-grafted polymer brushes.
Structural Characterization of an Exopolysaccharide from the Myxobacterium Sorangium Cellulosum NUST06
Jian Fa ZHANG , Xiang Hong XU , Hou Ming WU , Zhi Li LIU
2003, 14(1): 51-53
[Abstract](450) [FullText HTML] [PDF 1095KB](1)
Abstract:
The chemical structure of an exopolysaecharide (EPS) produced by Sorangium cellulosum NUST06 was investigated. The EPS was found to have molecular masses greater than 2×,106Da. and consisted ofD-glucose, D-mannose and D-glucuronic aeid in a ratio of 5:4:1. The analytieal results of methylation and nuelear magnetic resonance spectra suggested the EPS consist of following tetrasaeeharide repeating units:→4)-β-D-Glup-(1→4)-β-D-Glup-(1→4)-β-D-Glup-(1→???
Isolation and Characterization of an Antinicrobial Polypeptide from Loach
Xian Zhi DONG , Hui Bi XU , Kai Xun HUANG , Qiong LIU
2003, 14(1): 54-57
[Abstract](462) [FullText HTML] [PDF 1188KB](0)
Abstract:
A novel antimicrobial polypeptidc was isolated and charaeterized from loach, Misgurmis anguillieaudatus, The polypcptide, named MAPP, is a single-chain polypcptide with Mw about 9,800 Dalton and p1 about 4.78;the N-tag ofMAPP was CFGWN. MAPP showed good inhibition against various bacteria including Bacillus subtilis, Eseherichia coli and Staphylococcus aurens. MAPP could be used as a lead compound in antibiotics drug discovery.
A New Diterpenoid Dimer from Annona glabra
Nian Yun YANG , Li Juan TIAN , Zheng Mu MENG , Ying HAN
2003, 14(1): 58-61
[Abstract](454) [FullText HTML] [PDF 1067KB](2)
Abstract:
Anew diterpenoid dimer annonebinide A has been isolated from the stems ofAnnona glabra. Its structure was determined to be ent-16α-hydroxykauran-17-yl ent-16β-kauran-17-oate on the basis ofspectroscopic and chemical evidence.
Two New Ionone Derivatives from Rhododendron przewalskii Maxim
Guo Qiang LI , Zhong Jian JIA
2003, 14(1): 62-65
[Abstract](467) [FullText HTML] [PDF 1218KB](0)
Abstract:
Two new iononc derivatives, named rhododcndronc and rhododcndronsidc, were isolated from the alcoholic extract of the aerial parts of Rhododendron przwalskii Maxim. Their structures were elucidated on the basis of spectroscopic analysis
A New Acylated Flavonoid from Anaphalis aureo-punctata
Yan Qi WU , Shuo LI , Ya LI , Yu LI
2003, 14(1): 66-67
[Abstract](464) [FullText HTML] [PDF 566KB](1)
Abstract:
A new acylated tlavonoid glycoside, 3-O-kaempferol-3-O-acetyl-6-O-(P-coumaroyl)-β-D-glucopyranoside 1 was isolated from the whole plant of Anaphalis aureo-punctata. The structure was established by spectral methods.
Two New Taccalonolides from Tropic Plant Tacca subflaellata
Yue HUANG , A. MUEHLBAUER , T. HENKEL , Ji Kai LIU
2003, 14(1): 68-71
[Abstract](491) [FullText HTML] [PDF 1182KB](2)
Abstract:
Two new steroidal bitter principles, taccolanolide O, P have been isolated from Tacca subflaellata and their structures were established by spectroscopic methods.
DFT Study on One-carbon Unit Transfer from 1,10-CH+-tetrahydroquinoxaline to Methylamine
Chuan Song QI , Da Cheng FENG , Hua Yang WANG , Zheng Ting CAI
2003, 14(1): 72-75
[Abstract](524) [FullText HTML] [PDF 1459KB](1)
Abstract:
Density Funetional Theory (DFT) method was used in this paper to study one-carbon transfer from 1.10-tetrahydroquinoxalinc, an analoguc of tetrahydrofolic aeid, to methylamine.This reaetion can be completedvia two paths. From the computation result we can conclude thai a general-aeid catalysis exists in this reaction. By computation we find DFT has its limitation in deseribing a newly incorporated structure with a unit charge.
Two Lower-barrier Channels in the Reaction of HF with HOBO
Hai Tao YU , Yu Juan CHI , Hong Gang FU , Xu Ri HUANG , Ze Sheng LI , Jia Zhong SUN
2003, 14(1): 76-78
[Abstract](468) [FullText HTML] [PDF 874KB](0)
Abstract:
Two possible lower barrier reaction pathways in the reaction HF+HOBO→H2O+FBO are predicated by means of MP2 and CCSD(T) (single-point) methods. In the two channels, two stable intermediates are loeated and thus,they are multi-step channels,which are more favorable in energy than direct single-step reaction pathway predicated by previous theoretical study. Therefore,the two pathways should be main reaction channels in experiments.
Studies on Synthesis and Properties of Mg-Al-nitrate Layered Double Hydroxides
Qin Zheng YANG , Chun Guang ZHANG , De Jun SUN , Zhi Lin JIN
2003, 14(1): 79-82
[Abstract](478) [FullText HTML] [PDF 1302KB](1)
Abstract:
A positive Mg-Al-nitrate layered double hydroxides (LDHs) has been synthesized using a non-steady coprccipitation method. The shape, size, chemical composition, electrical property and anion exchange property of the positive nanoparticle were studied by SEM, XRD, FTIR,chemical analysis, spectroanalysis and measuring of electrophoretic mobilities. Preliminary results show the positive nanopartiele is a promising precursor ofpolymer/LDHs nanocomposite.
Solvothermal Route to Prepare the Metastable Phase 3c-Fe7S8 with Hexagonal Platelet Morphology
Xian Yun XU , Xiao Guang LI
2003, 14(1): 83-86
[Abstract](487) [FullText HTML] [PDF 1220KB](0)
Abstract:
The metastable phase 3c-Fe7S8 with the hexagonal platelct morphology has been prepared by using solvothcrmal routc. The product was charactcrized by means of X-ray powder diffraction (XRD) and transmission electron microscopy (TEM) and X-ray photoelcctron spectra (XPS). The experiment results show that the as-prepared Fe7S8 is a metastable phase with the hexagonal platelet morphology.
Direct Observation of Various Al Sites in SAPO-34 by 27Al Multiquantum (MQ) Magic Angle Spinning (MAS) NMR
Zhi Min YAN , Jian Qin ZHUANG , Lei XU , Xiu Wen HAN , Zhong Min LIU , Xin He BAO
2003, 14(1): 87-90
[Abstract](512) [FullText HTML] [PDF 1353KB](4)
Abstract:
The elegant 2D multiquantum (MQ) MAS NMR has been applied to invcstigatc the coordination of Al atoms in SAPO-34. The results show that the effects of the template and/or water on the coordination of Al atoms are significanl, which lead to the formation of various Al species. Up to four kinds of Al species are distinctly resolved.
Studies on the Recycling Efficiency of Thermoregulated Phase-separable Rh/PETPP Complex Catalyst
Yan Hua WANG , Fang CHENG , Xiao Wei WU , Zi Lin JIN
2003, 14(1): 91-93
[Abstract](500) [FullText HTML] [PDF 944KB](1)
Abstract:
Effects on the recycling effieieney of thermoregulated phase-separable Rh/PETPP (P-[p-C6H4O(CH2CH2O)nH]3, N=3n) complex catalyst involved in hydroformylation of 1-decene are for the first time presented. It was found that the loss of Rh is dependent greatly on the composition of phosphine ligand PETPP and the organic solvent employed in the reaetion.
One Novel Red-luminescent Coordination Polymer of Eu-p-ben-zenedicarboxylate with Nitrogen-donor-containing Lewis Base
Ming Zhao WANG , Jiang Bin XIA , Lin Pei JIN , Guan Liang CAI
2003, 14(1): 94-95
[Abstract](447) [FullText HTML] [PDF 696KB](0)
Abstract:
The crystal structure of novel coordination polymer with cxeellent charaeteristic luninescence of Eu3+, the three-dimentional network of {Eu2(p-BDC)3(Phen)2(H2O)2}n is presented.
Basic Functionalization of Hexagonal Mesoporous Silica
Chun YANG
2003, 14(1): 96-99
[Abstract](478) [FullText HTML] [PDF 1271KB](0)
Abstract:
3-Aminopropyltricthoxysilanc (AM), 3-cthyldiaminopropyltrimcthoxysilane (ED) and 3-piperazinylpropyltriethoxysilanc (PZ), were used to chemically couple with the silanol groups of calcined hexagonal and hexagonal-like mesoporous silica SBA-3 and HMS, respectively, to produce functionalised alkaline mesoporous materials. The inerease in the dosage of organosilanes, or in reaction temperature, or in the humidity (i.e., water content) of support, is favorable to the grafting of functional molecules on the surface. When functionalization conditions are the same, the order of loadings on SBA-3 and DDA-HMS is ED > AM > PZ. However, on ODA-HMS, the loading of AM is similar to that of ED.
Synthesis of Crystalline Nanosized Titanium Dioxide via a Reverse Micelle Method at Room Temperature
Dong Bai ZHANG , Li Min QI , Hu Min CHENG , Ji Ming MA
2003, 14(1): 100-103
[Abstract](501) [FullText HTML] [PDF 1441KB](0)
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Crystalline TiO2 nanoparticles were synthesized by hydrolysis of titanium tetrabutoxidein the presence of hydrochloric aeid in NP-5 (lgepal CO-520)/ cyclohcxane reverse micellesolution at room temperature. Pure rutilc nanoparticles were obtained at an appropriate acidconcentration. The influcnces of various reaction conditions such as the concentration of acids,water content value (w=[H2O]/[NP-5]) on the formation, crystal phase, morphology, and size of theTiO2 particles were investigated.
A Novel Heat-resisting Surfactant for the Modification of Alumina Nanoparticles
Yu Fen CHANG , Gui Ling NING , Yuan LIN , Chang Hou LIU , Yuan Bo LIN
2003, 14(1): 104-107
[Abstract](454) [FullText HTML] [PDF 1315KB](0)
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An easy preparation of controlled alumina nanoparticles by the solution precipitate method has been carried out using dendrimer as surfactant. The effects of the amount and size of surfactant on morphological control ofpowder have also been discussed.
Modification of Montmorillonite through Intercalative Polymerization
Lin Jie ZHI , Bing HAN , Tong ZHAO , Yun Zhao YU , Hong Sheng WANG
2003, 14(1): 108-110
[Abstract](477) [FullText HTML] [PDF 964KB](5)
Abstract:
Montmorillonite (MMT) was modified through intercalative polymerization of phenol and formaldchyde catalyzed by oxalic aeid. The modified montmorillonite was delaminated at large, as demonstrated by XRD and TEM studies. It can disperse easily in epoxy resin to form exfoliated nanocomp osites. The nanoscale silicate platclets dispersed in water can be metallized by silver deposition.
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