2004 Volume 15 Issue 10

New Condensation Reaction of β-keto-δ-valerolactones,Carbon Disulfide and Alkyl Halides
You Ming WANG , Yu Xin LI , Su Hua WANG , Zheng Ming LI
2004, 15(10): 1135-1136
[Abstract](202) [FullText HTML] [PDF 610KB](0)
β-Keto-δ-valerolactones, which were obtained by reaction of acetoacetate with aldehydes or ketones, reacted with carbon disulfide, alkyl halides and a new condensation reaction was developed. The structures of the products 3 were confirmed by 1HNMR spectra and elemental analysis.
A Green and Facile Solid-state Synthesis Method for the Preparation of Diazenecarboxamide Azo Compounds with Potassium Ferricyanide and Sodium Hydroxide System
Wan Xin XUE , Jian Ping LI , Yu Lu WANG
2004, 15(10): 1137-1139
[Abstract](202) [FullText HTML] [PDF 1162KB](0)
Eleven new-typed azo compounds were synthesized in good yields by dehydrogenating the corresponding aryl substituted semicarbazides using potassium ferricyanide and sodium hydroxide system under solid-state conditions.
Indium-mediated Facile Synthesis of (6-Chloropyridine-3-yl) methyl Heterocyclic Thioether Derivatives in Aqueous Media
Bao An SONG , Gang LIU , De Yu HU , Hua ZHANG
2004, 15(10): 1140-1142
[Abstract](201) [FullText HTML] [PDF 1158KB](0)
A series of substituted (6-chloropyridine-3-yl)methyl heterocyclic thioether derivatives were prepared by indium mediating in water. The preliminary biological tests showed that compound 3d exhibited good antiviral activity.
A Novel Method of Preparing Unsymmetrical Thioether from Disulfides
Jing Xing DU , Ren Wei ZHENG , Hong Yun GUO , Li Chun KONG
2004, 15(10): 1143-1145
[Abstract](202) [FullText HTML] [PDF 956KB](0)
The disulfides reacted with zinc in DMF, followed by alkyl halides, giving unsymmetrical thioether in excellent yields. This reaction takes place under mild and neutral conditions.
Efficient Esterification of Ferrocenecarboxylic Acid in Ionic Liquids
Wei Yi CHEN , Jun LU
2004, 15(10): 1146-1148
[Abstract](188) [FullText HTML] [PDF 916KB](0)
An efficient esterification of ferrocenecarboxylic acid with substituted phenols has been achieved using DCC/DMAP protocol in ionic liquids. The corresponding esters are produced in high yields.
A Mild and Efficient Oxidation of Alcohols in Water
Chuan Zhi XU , Lin CHEN , Zhen LI , Wei SUN , Chun Gu XIA
2004, 15(10): 1149-1152
[Abstract](198) [FullText HTML] [PDF 1233KB](1)
A mild and efficient oxidation of alcohols to the corresponding carbonyl compounds using the PhI(OAc)2(1.1 eq.) with n-Bu4NBr (8 mol%) in water at room temperature is described.This new procedure is very simple and affords the desired carbonyl compounds in high yields.
Synthesis and Crystal Structure of Triacetyltribenzyl-Hexaazaisowurtzitane (TATBIW·0.5 H2O)
Wei Rong HAN , Yu Xiang OU , Jin Quan LIU , Jian Long WANG
2004, 15(10): 1153-1156
[Abstract](219) [FullText HTML] [PDF 1421KB](2)
The compound of tetraacetyldibenzylhexaazaisowurtzitane (TADBIW) is an important precursor of synthesizing the high energetic dense compound of hexanitrohexaazaisowurtzitane (HNIW). We can obtain TADBIW by using hydrogenolysis of hexabenzylhexaazaisowurtzitane (HBIW). In the process of hydrogenolysis of HBIW, it will generate a variety of intermediates, one of them is the compound of triacetyltribenzylhexaazaisowurtzitane (TATBIW). We have synthesized the title compound and prepared its single crystal. In the paper, the crystal and molecular structure of TATBIW·0.5H2O is described. Its crystal belongs to the triclinie and space group P-1. The cell is comprised of two TATBIW and one water molecules. The success of synthesizing TATBIW can help us to research the mechanism of the reduction of HBIW and produce high yields of the end products.
Stereoselective Synthesis of (E)-1,3-Enynyl Bromides via Pd/Cu-catalyzed Cross-coupling Reaction of (Z)-α-Bromovinylstannanes
Ming Zhong CAI , Hong ZHAO
2004, 15(10): 1157-1160
[Abstract](192) [FullText HTML] [PDF 1418KB](0)
(Z)-α-Bromovinylstannanes undergo the cross-coupling reaction with alkynyl iodides in the presence of Pd(PPh3)4 and Cul in THF at room temperature to afford stereoselectively (E)-1, 3-enynyl bromides in good yields
Synthesis of Novel Monomeric Dyes with Anthraquinone Residue
Jing Xia WANG , Cheng You KAN , De Shan LIU
2004, 15(10): 1161-1163
[Abstract](193) [FullText HTML] [PDF 897KB](0)
Two novel polymerizable dyes with anthraquinone residue have been prepared, and their structures were characterized by FTIR, 1HNMR and EA.
A Concise Total Synthesis of S-(+)-Tylophorine
Zhong JIN , Shi Pu LI , Qing Min WANG , Run Qiu HUANG
2004, 15(10): 1164-1166
[Abstract](201) [FullText HTML] [PDF 916KB](2)
A highly efficient total synthesis of S-(+)-tylophorine has been accomplished in fully asymmetric fashion.
Simple,Mild and Convenient Synthesis of Two Novel N-Dichloro acetyl Oxazolidines and their Biological Activities
Chao CHAI , Fei YE
2004, 15(10): 1167-1169
[Abstract](187) [FullText HTML] [PDF 927KB](0)
Two N-dichloroacetyl oxazolidines were synthesized with a simple, mild and convenient method. All the compounds were characterized by IR, 1HNMR and elemental analysis. The preliminary biological test showed that the compounds protected maize against injury by some herbicides to some extent.
A Novel Green Synthesis of Quinolines through Acid-catalyzed Friedlander Reaction in Ionic Liquids
Xin Ying ZHANG , Xue Sen FAN , Jian Ji WANG , Yan Zhen LI
2004, 15(10): 1170-1172
[Abstract](183) [FullText HTML] [PDF 967KB](0)
Quinoline derivatives were efficiently prepared through acid-catalyzed Friedlander reaction in ionic liquid ([bmim] [BF4]). It is shown that the proposed method is operationally simple and environmentally benign in that the reaction media and the catalyst can be recovered and be reused effectively for at least four times.
Synthesis of Some Potential Antiangiogenic 1,3-Dihydro-1,3-dioxo 2H-isoindole Derivatives
Yong DENG , Yu YANG , Hui JIN , Yu Guo ZHONG
2004, 15(10): 1173-1176
[Abstract](189) [FullText HTML] [PDF 1785KB](0)
Based on the structure-activity relationships of RGD-containing peptides, a series of 1,3-dihydro-1,3-dioxo-2H-isoindole derivatives were synthesized. All of them were first reported.Their structures were confirmed by spectral data and elemental analysis. Their ability to inhibit angiogenesis were evaluated in the chick embryo chorioallantoic membrane assay at 10-5 mol/L.Compounds 5b and 5e displayed obviously antiangiogenic activity.
A Short and Stereoselective Synthesis of the (-)-(5R,6S)-6-Acetoxy hexadecane-5-olide
Bin SUN , Li Zeng PENG , Xue Song CHEN , Yu Lin LI , Ying LI
2004, 15(10): 1177-1178
[Abstract](188) [FullText HTML] [PDF 764KB](0)
(-)-(5R, 6S)-6-Acetoxyhexadecan-5-olide 1, a natural mosquito attractant pheromone,was synthesized from readily available aldehyde 2 and cyclopentanone 3 using L-proline-catalyzed asymmetric aldol reaction as the key step.
A New Triterpene from the Orchid Pholidota yunnanensis
Zhi Ming BI , Zheng Tao WANG , Luo Shan XU
2004, 15(10): 1179-1181
[Abstract](196) [FullText HTML] [PDF 902KB](0)
A new triterpene, 25-methylenecyclopholidonyl p-hydroxy-trans-cinnamate, was isolated from a orchid Pholidota yunnanensis. The structure elucidation and 1H, 13C-NMR assignments were achieved by spectral and chemical method.
Dihydrochalcones from Symplocos vacciniifolia
Tie Jun LING , Li Dong LIN , Ping WU , Wen Hua ZHOU , Hua Gu YE , Mei Fang LIU , Xiao Yi WEI
2004, 15(10): 1182-1184
[Abstract](193) [FullText HTML] [PDF 855KB](0)
A new dihydrochalcone glucoside, vacciniifolin, along with confusoside, trilobatin and sieboldin were isolated from the leaves of Symplocos vacciniifolia. By the method of spectra/analysis, this new compound was elucidated as 2',3,4,4'-tetrahydroxydihydrochalcone 4'-O-β-D-glucopyranoside.
A New Furobenzopyranone from Anaphalis lactea
Ai Xia WANG , Fu Lin YAN , Zhong Jian JIA
2004, 15(10): 1185-1186
[Abstract](186) [FullText HTML] [PDF 644KB](0)
A new furobenzopyranone, named anaphalisol, was isolated from the whole plant of Anaphalis lactea. Its structure was elucidated by spectroscopic methods including 2D NMR techniques.
Two New Tetranortriterpenoids from Amoora dasyclada
Shu Min YANG , Yun Bao MA , Xiao Dong LUO , Shao Hua WU , Da Gang WU
2004, 15(10): 1187-1190
[Abstract](188) [FullText HTML] [PDF 1260KB](1)
Two new tetranortriterpenoids 3-oxo-24, 25, 26, 27-tetranortirucall-7-ene-23(21)-lactone, 3α-hydroxy-24, 25, 26, 27-tetranortirucall-7-ene-23(21)-lactone were isolated from Amoora dasyclada. Their structures were elucidated by spectroscopic evidences.
A New Furostanol Saponin from the Water-extract of Dioscorea nipponica Mak.,the Raw Material of the Traditional Chinese Herbal Medicine Wei Ao Xin
Cheng Bin CUI , Chi XU , Qian Qun GU , Shi Dong CHU , Hai Hong JI , Gang JING
2004, 15(10): 1191-1194
[Abstract](196) [FullText HTML] [PDF 1530KB](1)
26-O-β-D-Glucopyranosyl-furost-5(6),20(22)-dien-3β,26-diol 1, a new furostanol saponin, was isolated from the water-extract of Dioscorea nipponica Mak., the raw material of a traditional Chinese herbal medicine Wei Ao Xin. The structure of 1 was determined on the basis of its spectral data especially by NMR spectroscopy. The result provides the first example of naturally occurring furostanol saponins with a single saccharide chain at the C-26 position.
A Novel Prenylchalcone from Humulus lupulus
Wen Shu WANG , Ya Wei ZHOU , Yun Hua YE , Mei Lan LI
2004, 15(10): 1195-1196
[Abstract](191) [FullText HTML] [PDF 565KB](0)
From hops of Humulus lupulus, a novel prenylchalcone was isolated, which showed inhibition against BGC-823 cells. The structure was elucidated as 5"-(2"'-hydroxyisopropyl-)-dihydrofurano-[2", 3"-B]-4, 4'-dihydroxy-6'-methoxychalcone, by HRFABMS and NMR spectra.
The Different Fluorescent Response of Quin 2 to the Binding of Ca2+ and La3+ and its Application
Jian HU , Xiao Da YANG , Kui WANG
2004, 15(10): 1197-1120
[Abstract](213) [FullText HTML] [PDF 1421KB](0)
The fluorescence spectra of Quin 2, (2-[(2-bis-[carboxymethyl] amino-5-methylphenoxy)methyl]-6-methoxy-8-bis[carboxymethyl] aminoquiniline), a Ca2+ probe, were investigated upon incubation with Ca2+ or La3+. The results showed that binding of La3+ to Quin 2 resulted in different fluorescent spectrum from that of Ca2+. Based on this observation, a fluorescent method was developed for simultaneously determination of the dissociation rates of Ca2+ and La3+ from a Ca-La-calmodulin complex (Ca2La2CaM).
A Novel Optical Properties of Molecular “Light Switch” and its Analytical Application
Fang CHEN , Jian Ping HUANG , Xin Ping AI , Zhi Ke HE
2004, 15(10): 1201-1204
[Abstract](191) [FullText HTML] [PDF 1323KB](0)
Because of the high affinity (KB ≥ 106 L mol-1) between Ru(phen)2(dppz)2+ and DNA, the adding of DNA in the solution of Ru(phen)2(dppz)2+-SDS makes the dissociation of Ru(pben)2(dppz)2+-SDS, and results in decrease of the resonance light scattering (RLS) signals and increase of the absorbance. Based on this, a novel method is proposed for DNA assay.
Protonation of 5,10,15,20-Tetra (4-hydroxyphenyl)-porphyrin in SDS Micellar Solution
Xiao Hong ZHAO , Yun Hong ZHANG
2004, 15(10): 1205-1208
[Abstract](209) [FullText HTML] [PDF 1477KB](0)
An amphiphilic porphyrin, 5, 10, 15, 20-tetra(4-hydroxyphenyl)-porphyrin (P) was solubilized in SDS micellar solutions. By taking advantage of protonation property of pyridine groups of amphiphilic porphyrin and the UV-Vis spectral sensitivity of Soret band and Q bands to the microenvironment of the porphyrin moiety, two-step protonation was studied in detail by means of UV-Vis spectroscopy. The free base, monocation and dication were described in detail in SDS micellar solution. The possibility of microphase transition was proposed to relate to the observation of two isosbestic points.
Enantiomeric Separation of Epinephrine and Salbutamol by Micellar Electrokinetic Chromatography Using β-Cyclodextrin as Chiral Additive
Yan Peng ZHENG , Jin Yuan MO
2004, 15(10): 1209-1211
[Abstract](201) [FullText HTML] [PDF 827KB](0)
Enantiomeric separation of epinephrine and salbutamol was investigated by micellar electrokinetic chromatography employing β-cyclodextrin as chiral additive in ammonium chloride-ammonia solution. The analytes were detected by electrochemistry using gold microelectrode at +0.65 V versus SCE reference electrode. The effects of detection potential,concentration of β-cyclodextrin, concentration of sodium dodecyl sulfate, pH value of electrolyte and applied voltage were discussed.
Beaded Fiber Mats of PVA Containing Unsaturated Heteropoly Salt
Guo Cheng YANG , Yan PAN , Jian GONG , Chang Lu SHAO , Shang Bin WEN , Chen SHAO , Lun Yu QU
2004, 15(10): 1212-1214
[Abstract](198) [FullText HTML] [PDF 1192KB](0)
Poly(vinyl alcohol) (PVA) fiber mats containing unsaturated heteropoly salt was prepared for the first time. IR, X-ray diffraction and SEM photographs characterized the beaded fiber mats.The viscoelasticity and the conductivity of the solution were the key factors that influence the formation of the beaded fiber mats.
Effects of the Liquid Conductivity on Pulsed High-voltage Discharge Modes in Water
Bin YANG , Le Cheng LEI , Ming Hua ZHOU
2004, 15(10): 1215-1218
[Abstract](188) [FullText HTML] [PDF 1637KB](0)
Spark, stream and corona pulsed high-voltage discharges in water induced by the various initial conductivities have been examined in this paper. The discharge modes changed from spark to corona discharge with the liquid conductivity increasing. The apparent production of OH radical and quantum yield generated by spark discharge in distilled water were 11.57 μmol/L and 0.0978photon/s, respectively. A preliminary study on acid fuchsine (AF) treatment indicated that higher AF removal efficiency has been achieved by spark discharge. The process of degradation showed that the oxidative effects through OH radical oxidation did not play an important role and did increase with the discharge mode changing to spark discharge.
Extraction of Cesium from the Irradiated Nuclear Waste by 4(5),4'(5')-Bis[1-hydroxyalkylbenzo]-21-crown-7
Ying DU , Wen Jun CHEN , Sheng Ying QIN
2004, 15(10): 1219-1222
[Abstract](191) [FullText HTML] [PDF 1248KB](0)
4(5),4'(5')-Bis[l-hydroxyalkylbenzo]-21-crown-7 (A-C) have been synthesized by two-step reactions from dibenzo-21-crown-7 (DB21C7). Extraction of cesium cation from nitric acid solutions by A-C has been investigated in nitromethane. Under the conditions of various concentration of HNO3 or NaNO3, the extractabilities of A and B were superior to that of DB21C7.
Green Oxygenation Degradation of Rhodamine B by Using Activated Molecule Oxygen
Ke Jian DENG , Fei HUANG , Duo Yuan WANG , Zheng He PENG , Yun Hong ZHOU
2004, 15(10): 1223-1226
[Abstract](204) [FullText HTML] [PDF 1648KB](0)
Iron(Ⅱ) tetra-(1,4-dithin)-porphyrazine, (FePz(dtn)4) is able to activate molecule oxygen for oxygenation degradation of rhodamine B (RhB) in an extensive pH region without light excitation. Experiments indicate that the RhB can be degraded nearly 52% in alkaline aqueous solution, bubbling with dioxygen for seven hours in the presence of FePz(dtn)4 and the hydrogen peroxides as an actve intermediate were determined by DPD method. The catalyst is recyclable and the catalyst activity was maintained after l0 recycles.
Fabrication of Layer-by-layer Films of Polyhedral Oligomeric Silsesquioxanes
Xiao Meng WANG , Han Ming DING , Yong Kui SHAN , Ming Yuan HE
2004, 15(10): 1227-1229
[Abstract](192) [FullText HTML] [PDF 1222KB](0)
Layer-by-layer (LBL) self-assembly method was used to fabricate siliceous ultrathin films by using polyhedral oligomeric silsesquioxanes as building blocks. Ammonium salt of octasilsesquioxane acid (OSi8) and poly(diallyldimethylammonium chloride) (PDDA) were alternately assembled onto CaF2 slide to form nanocomposite multilayers. Linear build-up of the LBL films was confirmed by UV-Vis spectroscopy. IR spectrum suggests existence of OSi8 and PDDA in the LBL films. Atomic force microscopic surface topography of the LBL films indicates the OSi8 covers the entire surface of the topmost layer and shows a granular morphology.
Novel Carbon Nanotubes-supported NiB Amorphors Alloy Catalyst for Benzene Hydrogenation
Mei Hua YANG , Rong Bin ZHANG , Feng Yi LI
2004, 15(10): 1230-1232
[Abstract](190) [FullText HTML] [PDF 1193KB](0)
The NiB amorphous alloy catalysts supported on CNTs and alumina were prepared by impregnation and chemical reduction. The gas-phase benzene hydrogenation was used as a probe reaction to evaluate the catalytic activity. The result showed that the NiB amorphous alloy catalyst supported on carbon nanotubes exhibited higher activity than that supported on alumina.
Covalently Attached Monolayer of Phthalocyanine on Chemically Modified Silicon Oxide Surface
Quan ZHOU , Hong Zheng CHEN , Jing Zhi SUN , Mang WANG , Duan Lin QUE
2004, 15(10): 1233-1236
[Abstract](201) [FullText HTML] [PDF 1402KB](0)
Highly stable monolayers of 2,9,16,23-tetracarboxyl phthalocyanine on 3-aminopropyl-triethoxysilane (ATS) modified silicon and quartz substrates were prepared by reaction of carboxyl and amine. The monolayers were characterized by UV-Vis spectra and AFM measurements. The results indicated that the ultra-thin films on silicon or quartz were smooth, and the ordered structures were observed in these films.
Studying Aggregate in Lysozyme Solution by Atomic Force Microscope
Guo Liang DAI , Yong YU , Qi KANG , Wen Rui HU
2004, 15(10): 1237-1240
[Abstract](181) [FullText HTML] [PDF 1615KB](0)
The aggregates in lysozyme solution with different NaCl concentration were investigated by Atomic Force Microscope (AFM). The AFM images show that there exist lysozyme monomers,n-mers and clusters in lysozyme solution when the conditions are not suitable for crystal growth. In favorable conditions for crystal growth, the lysozyme clusters disappear and almost only monomers exist in solution.
Clean Aerobic Liquid Oxidation of Aldehydes with Solid Catalyst
Hong Bing JI , Du Gui HE , Jun SONG , Yu QIAN
2004, 15(10): 1241-1244
[Abstract](185) [FullText HTML] [PDF 1685KB](0)
Clean liquid oxidation of aldehydes can be accomplished using solid catalyst in the presence of molecular oxygen at room temperature, which is a valuable alternative to traditional counterparts.
Photopromoted Methoxycarbonylation of Olefins Under Ambient Conditions in DMF
Wen Hao SUN , Jing Mei YIN , Da Bin GAO , Guang Yun ZHOU , Ying Ping JIA , Xiang Sheng WANG
2004, 15(10): 1245-1248
[Abstract](208) [FullText HTML] [PDF 1319KB](0)
Photopromoted methoxycarbonylation of olefins with carbon monoxide can be carried out under ambient conditions with non-precious transition metal complexes (such as cobalt complexes) catalysts in DMF. The isotope experiments show that DMF is decomposed under irradiation and is conveniently used as a carbon monoxide source for the reaction.
Selenium Nanoparticles Prepared from Reverse Microemulsion Process
Ming Zhu LIU , Sheng Yi ZHANG , Yu Hua SHEN , Ming Liang ZHANG
2004, 15(10): 1249-1252
[Abstract](181) [FullText HTML] [PDF 1880KB](1)
Selenium nanoparticles were prepared by a reverse microemulsion system. Sodium selenosulfate was used as selenium source. The results showed that hydrochloric acid concentration and reaction temperature had great influence on the morphology of products. The crystalline selenium nanowires and amorphous selenium nanorods were obtained in given condition.
The Preparation and Properties of Thermosensitive Hydrogels Based on Chitosan Grafted N-isopropylacrylamide via γ-Radiation
Hong CAI , Jing ZHANG , Zheng Pu ZHANG , Yan Geng ZHANG , Bing Lin HE
2004, 15(10): 1253-1254
[Abstract](170) [FullText HTML] [PDF 596KB](0)
Thermosensitive hydrogels were prepared by graft polymerization of chitosan and N-isopropylacrylamide via 60Co γ-radiation. The effects of monomer concentration and total irradiation dose on percent grafting and grafting efficiency were studied. The thermosensitivity and swelling properties of the hydrogels were investigated.
Synthesis of a New Polyoxometalate Loaded Stearic Acid Nanoparticles
Yong YANG , Lei ZHANG , Wei FAN , Xiao Hong WANG , Bin LI , Jing Fu LIU
2004, 15(10): 1255-1257
[Abstract](165) [FullText HTML] [PDF 1074KB](1)
The stearic acid nanoparticles loaded polyoxometalate K6[γ-(CpTi)2SiW10O38] [(CpTi)2SiW10] have been prepared and structurally characterized by elemental analysis, IR spectra.The particle size was estimated by transition electron microscope and zatesizer instrument. The result showed that the polyoxometalate retained the parent structure after encapsulation by stearic acid nanoparticles.
A SAPO-11 Silicoaluminophosphate Molecular Sieve with Stable Crystal Structure
Yue Ming LIU , Feng Mei ZHANG , Hai Hong WU , Hai Jiao ZHANG , Jian Guo YANG , Xing Tian SHU , Ming Yuan HE
2004, 15(10): 1258-1260
[Abstract](213) [FullText HTML] [PDF 1195KB](0)
A SAPO-11 silicoaluminophosphate molecular sieve with stable crystal structure was synthesized for the first time. After removing template by calcination, its crystal space group still retains Icm2 which the as-synthesized has. The catalyst deriving from the present SAPO-11materials shows higher isomerization selectivity and higher paraffin hydroisomerization yield than those reported elsewhere.
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