1997 Volume 8 Issue 6

The Reaction of Benzimidazole Methiodide Salt with Bis-Grignard Reagent
Zhen SHI , Huan GU
1997, 8(6): 465-466
[Abstract](200) [FullText HTML] [PDF 63KB](0)
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The reaction of benzimidazole methoidide salt with bis-Grignard reagent is reported,and a new method for the preparation of dialdehyde is provided.
Studies on the Reaction of Vinyl Triazole Derivatives with Hydroxylamine
Gui Yu JIN , Guo Feng ZHAO , Zhong Fa LIU , Jin REN , Yu Chang LI
1997, 8(6): 467-470
[Abstract](190) [FullText HTML] [PDF 162KB](0)
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In this paper the reaction of vinyl triazole denvatives with hydroxylamine hydrochloride under the action of sodium carbonate was studied.The result indicated that cyclization took place and new heterocyclic compounds of 1,2-oxazocyclopentanes were obtained.
Novel Reduction of Arylsulfonyl Chlorides and Sodium Alkyl Thiosulfates to Disulfides with TiCl4/Zn System
Zhuang Pin ZHAN , Hong Yun GUO , Yong Min ZHANG
1997, 8(6): 471-472
[Abstract](196) [FullText HTML] [PDF 85KB](0)
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TiCl4/Zn system reduces arylsulfonyl chlorides and sodium alkyl thiosulfates to corresponding disulfides in moderate to good yields.
The New Synthesis of Azo Urea from Substituted Semicarbazide
Xiao Yang WANG , Yu Lu WANG , Jian Ping LI , Cai Lan WANG , Hong WANG
1997, 8(6): 473-474
[Abstract](192) [FullText HTML] [PDF 108KB](0)
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Using N-bromosuccinimide and pyridine as the oxidation system to dehydrogenate aryl substituted semicarbazide to form azo compounds is described for the first time in this paper.Nine azo compounds have been prepared in excellent yield under mild condition.This method only needs simple instrument and short reaction time.
Synthesis and Binding Properties of Novel Cyclodextrin Dimers Linked at C-6 by the Shortest Bridge-a Sulfur Atom
De Qi YUAN , Kahee FUJITA , Yuji OKABE
1997, 8(6): 475-476
[Abstract](200) [FullText HTML] [PDF 107KB](0)
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Three cyclodextrin dimers bridged at C-6 by the shortest tether-a sulfur atom are synthesized by reacting cyclodextrin tosylates with Na2S and their binding properties are evaluated.
Enantioselective Hydrogenation of α,β-Unsaturated Cyclic Ketones by Double Asymmetric Induction Preparation of (R)-Muscone
Bao Han XIE , Shi Jie LU , Hong Xiang FU , Lan Yong GAO
1997, 8(6): 477-478
[Abstract](209) [FullText HTML] [PDF 76KB](1)
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By ketal formation with chiral glycols like methyl or ethyl ester of tartaric acid,hydrogenation of ketals from the corresponding α,β-unsaturated 15-membered cyclic ketone produces (R)-muscone in good chemical and optical yield in the presence of chiral catalysts.
Study on the Mechanism of the Rearrangement Reaction of 3-n-Butylphthalide by Deuterium-Labelling
Bai Ling XU , Zong Ru GUO , Xiao Tian LIANG , Guang Zhong YANG
1997, 8(6): 479-482
[Abstract](198) [FullText HTML] [PDF 148KB](0)
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By the Grignard reaction of 1,1-di-deutero-1-bromobutane with phthalaldehydic acid 1',1'-di-deutero-3-n-butyl phthalide was obtained.which underwent a rearrangement reaction using AlCl3 as catalyst in CS2 to give 1-methyl-5-carboxy-3,4-di-deutero-tetrahydronaphthalene.The mechanism was proposed to be a series of consecutive 1,2-hydride transfers rather than a direct 1,4-hydride transfer.
Synthesis of Novel Molecular Receptors from Estradiol Dimer
Dong Hong LI , Dong Chuan SHI , Shu Hua CHEN , Hua Ming ZHAO
1997, 8(6): 483-486
[Abstract](172) [FullText HTML] [PDF 145KB](0)
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A novel type of estrogen-based receptor has been synthesized.These receptor compounds 3a-d have been characterized by mass spectra,1H NMR spectra,IR spectra and elemental analyses.
A Facile Convergent Approach to Octopus Polyestrone
Ying Chun CHEN , Ling Ling WENG , Hu ZHENG
1997, 8(6): 487-490
[Abstract](173) [FullText HTML] [PDF 114KB](0)
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Dendrimers have attracted attention in abroad area of chemistry.In this paper,octopus polyestrones were easily synthesized in a novel convergent strategy.
Studies on Agarofurans Ⅱ.Stereoselective Synthesis of 1α-and 1β-Methyl Agarofuran
Wu Yan ZHANG , Ji Yu GUO , Xiao Tian LIANG
1997, 8(6): 491-492
[Abstract](726) [FullText HTML] [PDF 110KB](0)
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1α-and 1β-methyl agarofuran 1 and 2 were stereoselectively synthesized,the key intermediates being synthesized through stereoselective Robinson annulation.The conjugated double bond was reduced in an improved way.Alkylation of imine 7 with enone 8,9,10 was performed.
Studies on the Crinum Alkaloids part Ⅱ[1]:Synthes is of Crinasiadine and Trisphaeridine
Hua Wu SHAO , Jun Chao CAI
1997, 8(6): 493-496
[Abstract](164) [FullText HTML] [PDF 106KB](1)
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Crinasiadine 1 has been easily synthesized by palladium acetate catalyzed cyclization of N-(o-bromophenyl)-3,4-methylenedioxybenzamide.The synthesis of trisphearidine 8 with a practical type of palladium chloride catalyzed cyclization as the key step is reported.
Synthesis of Novel Fluorine-Containing Surfactants Using Aleuritic Acid as a Starting Material
Jin YANG , Jin Tao LIU , Ji Qing YAANG , Wei Yuan HUANG , Jing Yuan LI
1997, 8(6): 497-498
[Abstract](185) [FullText HTML] [PDF 93KB](0)
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A novel type of fluorine-containing surfactants 5 was synthesized using aleuritic acid as a starting material in six steps with an overall yield of 9%.
Novel Zwitterionic Surfactants:Synthesis and Surface Active Properties of N-(3-Alkoxy-2-Hydroxypropyl)-N, N-Dimethyl glycine Betaines
Jing Qu GUAN , Xi You LI , Chen Ho TUNG
1997, 8(6): 499-502
[Abstract](167) [FullText HTML] [PDF 136KB](0)
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Five new zwitterionic surfactants with long chain alkyl betaine structure incorporated with hydroxylpropyl group have been synthesized.Their structures were identified by elemental analysis,IR,1HNMR,and 13CNMR.Surface tension experiments showed that these surfactants have higher surface activity than those without hydroxypropyl group.The values of CMC and γCMC of these surfactants have been determined.
Comparative Molecular Field Analysis on a Set of New Herbicidal Sulfonylurea Compounds
Jie LIU , Xia WANG , Yi MA , Zheng Ming LI , Cheng Ming LAI , Guo Feng JIA , Ling Xiu WANG
1997, 8(6): 503-504
[Abstract](169) [FullText HTML] [PDF 84KB](0)
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In this paper Comparative Molecular Field Analysis (CoMFA) method was applied to study the three-dimensional quantitative structure activity relationship (3D-QSAR) on a set of new herbicidal sulfonylureas.We optimized molecular structures to improve their activities.
Predictions of Reactivities of the Outer-Sphere Electron Exchange Reactions in Solution
Zheng Yu ZHOU , Jian XU
1997, 8(6): 505-508
[Abstract](167) [FullText HTML] [PDF 152KB](0)
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One of the crucial parameters determining the electron transfer rate,Franck-Condon factor,was evaluated quantitatively for electron exchange reactions involving hexaquo-metal ions.Adopting appropriate spectroscopic and photoemission data,reasonable results were obtained and compared in terms of classical and quantum-mechanical theory.Investigation shows that for such reactions occurred at room temperature,nuclear tunneling effects increase the absolute rates by several times,which are not dramatic but still should be considered for complementary purpose.
Gnetifolin K,a New Stilbene Diglucoside from Gnetum parvifolium
Qun XU , Mao LIN
1997, 8(6): 509-510
[Abstract](180) [FullText HTML] [PDF 94KB](0)
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A new stilbene diglucoside,gnetifolin K.was isolated from the lianas of Gnetum parvifolium.Its structure was established as isorhapotigenin-3,4'-di-O-β-D-glucoside on the basis of spectral and chemical evidence.
Four New Steroidal Alkaloids from the Roots of Sarcococca Vagans
Shi Shan YU , Zhong Mei ZOU , Jie ZEN , De Quan YU , PU Zhu CONG
1997, 8(6): 511-514
[Abstract](174) [FullText HTML] [PDF 200KB](0)
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Four new steroidal alkaloids,named sarcovagine A-D,were isolated from the roots of Sarcococca vagans.Their structures were determined as 20α-dimemylamino-2β,4β-dihydroxy-3β-tigloylamino-5α-pregnane (sarcovagine A,1),20α-dimethylamino-2α-hydroxy-4β-acetoxy-3β-tigloylamino-5α-pregnane (sarcovagine B,2),20α-dimethylamino-4β-acetoxy-3β-tigloylamino-5α-pregnane (sarcovagine C,3),20α-dimemylamino-3-tigloylamino-5α-pregn-2(3)-en-4-one (sarcovagine D,4),respectively.
Identification of the Metabolite of 7-(4-Chlorbenzyl)-7,8,13,13a-tetrahydroberberine chloride in Rat Bile by LC/MS and LC/NMR
Nian Ping FENG , Zheng Xing ZRANG , Deng Kui AN , Wen Long HUANG , Guang Ji WANG , Xiu Wen HAN , Xin He BAO
1997, 8(6): 515-518
[Abstract](179) [FullText HTML] [PDF 89KB](2)
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The metabolism of 7-(4-Chlorbenzyl)-7,8,13,13a-tetrahydroberberine chloride (CTHB),a potential anti-arrhythmia and anti-ischemia drug,was studied in rat bile.A metabolite and unchanged CTHB were found in the bile.Characterization and structural elucidation of the metabolite was achieved by LC/MS and LC/NMR.
Preparation and Characterization of Bonded Stationary Phase Containing Monoaza Crown Ether for High-Performance Liquid Chromatography
Jin Mao YOU , Guo Huang XIE , Hong En WANG , Guo Jun WANG , Chang Li ZHOU , Ji Xin SU
1997, 8(6): 519-522
[Abstract](173) [FullText HTML] [PDF 164KB](0)
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Silica gel bonded stationary phases containing monoaza crown ether was synthesized via a series of solid-liquid phase reactions.The bonded molecular structure was characterized by chemical and instrumental analyses.The bonded stationary phase was provided with complexing ability with copper ion as well as hydrophobic property.The chromatographic retention behaviours of some substituted polar phenol derivatives,organic acids and bases on the bonded stationary phase were studied using methanol and/or aqueous solution of dibasic potassium phosphate buffer as mobile phase.When copper ion was added to the mobile phase at pH 5.4.the retention of substituted phenols became strong.
Interaction between Cationic Surfactants and Bromopyrogallol Red as well as Its Application for the Sensitive and Selective Determination of Mo in Mo/W Binary Mixtures
Xi Rong HUANG , Shu Hua HAN , Wen Juan ZHANG , Yong Quan YIN , Gui Ying XU
1997, 8(6): 523-526
[Abstract](179) [FullText HTML] [PDF 146KB](0)
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Prior to formation of the micelles of cationic surfactant (CSF),bromopyrogallol red (BPR) could exist in the forms of both monomer and oligomer.After that,however,only BPR monomer existed.Nonionic surfactant OP-10 favoured the oligomerization of BPR monomer.The mixed micellar media prepared by mixing CSF and OP-10 in an appropriate ratio could be used for the sensitive and selective determination of Mo in Mo/W binary mixtures.
Dual Differential Thermal Analysis and Instrument
Zuan Guang CHEN , Peng LIU , Min Sheng ZRANG
1997, 8(6): 527-528
[Abstract](163) [FullText HTML] [PDF 120KB](0)
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A new method of differential thermal analysis and instrument were developed.The solution and pure solvent were placed in a cooling bath whose temperature was decreased by a semiconductor chip.Three detectors were used to sense the temperature (Ts,Tr and Tw) of solution (S),pure solvent (R) and cooling bath (W).When (Tr-Ts)-(Ts-Tw) presented maximum,(Tr-Ts) was the freezing point depression of the solution which was proportional to the concentration of solution.An instrument for the method was designed.
Adsorptive Stripping Voltammetric Study of the Enhancement of Copper(Ⅱ) by Poly (vinyl alcohol),Starch and Polyallylamine
Ming SONG , Hui Min MA , Yue Xian HUANG , Shu Quan LIANG
1997, 8(6): 529-532
[Abstract](174) [FullText HTML] [PDF 158KB](0)
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Adsorptive enhancements of several water-soluble polymers on copper(Ⅱ) were studied by adsorptive stripping voltammetry with a hanging mercury drop electrode.Increases in peak current of Cu(Ⅱ) were observed in alkaline carbonate media.The enhancing power of poly(vinyl alcohol),starch and polyallylamine is 15,4.1,and 2.5 times,respectively.
EQCM study on poly(aminothiophenol) monolayer
Qing Ji XIE , Ming MA
1997, 8(6): 533-534
[Abstract](168) [FullText HTML] [PDF 107KB](0)
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In this letter,we report EQCM studies on the electrochemistry of poly(aminothiophenol) monolayer on Au in aqueous solutions.Results show that the monolayer polymer investigated exhibits only a one-step proton-involving redox process without doping and undoping behaviors similar to polyaniline.
Study on Electrophotographic Properties for Dual Layered Photoreceptor
Shu qin ZHOU , Xiao dong DENG
1997, 8(6): 535-538
[Abstract](173) [FullText HTML] [PDF 164KB](0)
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One kind of dual layer function separated architecture photoreceptors was prepared.As compared with that of single layered photoreceptor made of the same photogenerator material,their absorption spectra and electrophotographic properties were investigated systematically.The experimental results indicate that phthalocyanine compounds are appropriate photogenerators.The existence of CTL in the dual layered photoreceptor efficiently accelerated photodecay process and bring about a lower Vr value,and higher light sensitivity than that of single layered photoreceptor.These are attributed to carrier injection from CGL to CTL.The process might be interpreted as assistance sensitization effect based on carrier injection.It might play an important role in promoting the performance of dual layered photoreceptor.
Vesicle Formation from Equimolar Cationic-anionic Surfactant Mixture in Non-aqueous Media
Guo Xi ZHAO , Zhen Le YANG , Bu Yao ZHU
1997, 8(6): 539-542
[Abstract](173) [FullText HTML] [PDF 287KB](0)
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Unilamellar vesicles from the mixtures of 1:1 sodium 10-undecenoate and trimethyl[2-(10-undecenoyloxy) ethyl] ammonium iodide in the mixed solvents of ethanol and heptane can be formed spontaneously or by sonication.They can exist in the variation of concentrations and volume ratios of ethanol to heptane,which indicates to some extent the high capability of vesicle formation in such mixed systems.
Critical Transitions of Microviscosity in Concentrated Polystyrene Solutions Revealed by Excimer Formation of Pyrenyl Probes
Huan GAO , Guo Chang WANG , Bing Lin HE
1997, 8(6): 543-546
[Abstract](165) [FullText HTML] [PDF 125KB](0)
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Excimer formation of pyrene and benzyl 4-(1-pyrenyl) butanoate was used to study the microviscosity of polystyrene/toluene solutions over the entire concentration range.Two critical concentrations (CPS~0.32,0.82g/ml) have been observed from the log-log plot of IE/IM vs CPS.The results are explained in terms of the onset of cohesional interaction and the glass transition of the polymer chains,respectively.
Nonheme Oxovanadium (Ⅴ,Ⅳ) Complexes Catalyze the Oxidative Cleavage of Catechols
Bo Yan ZHANG , Yi ZHANG , Bao Wei CHEN , Kui WANG
1997, 8(6): 547-550
[Abstract](167) [FullText HTML] [PDF 177KB](0)
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It was found that the oxovanadium (V) complex of triethanolamine (TEA) exhibits catalytic activity to the oxidative cleavage of catechols.On the other hand,the vanadyl nitrilotriacetic acid (NTA) complex is inactive.but leads to the formation of stable ternary complex.The main products of the catalytic oxidative cleavage of 3.5-di-tert-butylcatechol were separated and characterized.Based on the results,a reaction mechanism was discussed.
The Interaction of Cobalt (Ⅲ) Mixed-Ligand Coordination Compound Containing Dipyrido[3,2-a:2',3'-c] phenazine With Calf Thymus DNA
Lan JIN , Pin YANG
1997, 8(6): 551-552
[Abstract](179) [FullText HTML] [PDF 471KB](0)
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The binding of Co(phen)2dppz3+ to calf thymus DNA was investigated using absorption spectroscopy,viscosity and electrophoresis measurements,where dppz is dipyrido[3,2-a:2'3'-c] phenazine.The compound shows absorption hypochromicity and the specific viscosity increased upon binding to calf thymus DNA.The complex is also shown to be more efficient photosensitisers for single strand breaks in plasmid DNA.
A Facile Synthesis of Manganese Porphyrin Thiolates
Lin Jing MU , Yong Qia ZHOU , Jie Sheng HUANG , Pan Wen SHEN
1997, 8(6): 553-554
[Abstract](161) [FullText HTML] [PDF 106KB](0)
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The attractive and important complexes,manganese porphyrin aromatic thiolates,are prepared directly by the reaction of chloro(5,10,15,20-tetraphenylporphyrinato) manganese Mn(TPP)Cl with PhSNa and (p-NO2)PhSNa under extremely simple and mild reaction conditions.
Synthesis and Magnetism of μ-IsophthalatoOxovanadium(Ⅱ) Binuclear Complexes
Cui Wei YAN , Yan Tuan LI , Dai Zheng LIAO
1997, 8(6): 555-556
[Abstract](170) [FullText HTML] [PDF 79KB](0)
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Two μ-isophthalato oxovanadium (Ⅱ) binuclear complexes,[(VO)2-(IPHTA)(phen)2]SO4 (1) and [(VO)2(IPHTA)(NO2-phen)2]SO4 (2) were synthesized and characterized.The magnetism of complex (1) was studied.
Synthesis and Characterization of Dipeptide Schiff Base Complexes of Copper(Ⅱ), Zinc(Ⅱ), Nickel(Ⅱ) and Cobalt(Ⅱ)
Guang Bin WANG , Jin Ling WANG , Fang Ming MIAO
1997, 8(6): 557-558
[Abstract](170) [FullText HTML] [PDF 104KB](0)
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A new Schiff base (LK) obtained from 2,4,-dihydroxybenzaldehyde and glycyl-DL-phenylalanine reacted with Cu(Ⅱ),Zn(Ⅱ),Ni(Ⅱ) and Co(Ⅱ) to yield new complexes.The complexes were characterized by elemental analyses,molar conductance,1H NMR,DTA,TG,BR and UV spectroscopy.In these complexes the ligand is coordinated to the metal through its phenolic oxygen,carboxyl oxygen,imino nitrogen and amide nitrogen.All complexes are non-electrolytes and four-coordinated with 1:1 (metal:ligand) stoichiometry.The probable structure of the complexes is suggested.
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