1997 Volume 8 Issue 1

Facile Synthesis of trans-3,4-Diol Derivatives of Substituted Chromans via Catalytic Epoxidation
Hong Bin SUN , Zheng YAN , Wei Yi HUA , Wen Long HUANG , Si Xun PENG
1997, 8(1): 1-4
[Abstract](163) [FullText HTML] [PDF 178KB](0)
A practical synthesis of trans-3,4-diol derivatives of substituted chromans via epoxidation with combined use of mangenese (Ⅲ) salen complex 3 and hydrogen peroxide has been developed.These diol derivatives are key intermediates for the synthesis of a series of biologically important chroman compounds.
Synthesis of 1H-thiopyrano [3,4-b] Quinolin-4(3H)-one and Their Heterocycle Fused Compounds
Yong Jun GAO , Feng Jun LI , Ri Shan JIANG , Shi Chen ZHOU
1997, 8(1): 5-6
[Abstract](160) [FullText HTML] [PDF 91KB](0)
1H-Thiopyrano[3,4-b] quinolin-4(3H)-one 1,a new series of heterotricyclic ketone and their heterocycle fused compounds (2 and 3) were prepared by a simple procedure in good yields.
The Intramolecular Coupling Reaction of 1,6-Bis(1-Alky1-2-Methylindol-3-yl)hexane-1,6-dione Induced by Low-valent Titanium
Zhen Nian HUANG , Sheng JIN , Mei Gong FAN
1997, 8(1): 7-8
[Abstract](166) [FullText HTML] [PDF 81KB](0)
The intramolecular reductive coupling reaction of 1,6-bis(substituted indolyl)hexane-1,6-dione using zero-valent titanium reagent as catalyst produces the novel photochromic 1,2-diheterocyclic cyclohexenes 2,together with unexpected compounds 3.
Synthesis of New Germanium Compounds Containing α-Amino AcidEster or α-Phosphonate Groups
Zhong Biao ZHANG , Lian Sheng LI , Ru Yu CHEN , Qing Min WANG , Qiang ZENG
1997, 8(1): 9-10
[Abstract](174) [FullText HTML] [PDF 65KB](0)
A series of new type of germasesquioxides.germatranes,and β-trichlorogermylpropionic acid derivatives containing α-amino group or α-aminophosphonyl group were synthesized by a convenient condensation reaction of β-trichlorogermyl propionyl chloride with α-amino acid esters or α-phosphonates in the presense of organic base.The structures of products were determined by 1HNMR.31PNMR,IR,MS,elemental analysis,and X-ray diffraction.
Synthesis and Stereochemistry of New Cyclic Phosphate-phosphonates
1997, 8(1): 11-12
[Abstract](172) [FullText HTML] [PDF 107KB](0)
The novel cyclic phosphate-phosphonates,cis/trans-2-phosphonobenzyloxy-4-aryl-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-sulfides(selenides) (7a-f),were synthesized by a one-pot reaction using tris(diethylamino) phosphine activated by iodine as the phosphorylating and ring-closing reagent in good overall yields.The geometric stereoisomers were isolated and characterized.A cis-configuration and a chair preferred conformation of one isomer of 7b were established by X-ray diffraction analysis.
An Efficient and Stereoselective Synthesis of (-)-Massoialactone
Chi ZHANG , Fang Ning ZHANG , Xue Chao WANG , Yu REN , Xin Fu PAN
1997, 8(1): 13-14
[Abstract](162) [FullText HTML] [PDF 72KB](0)
An efficient and stereoselective four step synthesis of (-)-Massoialactone (1) is described .The key step involves deoxygenation of one α,β-unsaturated carbonyl group in compound 5.
Study on the Total Synthesis of Hainanolide(Ⅱ)——An Unexpected Hydroperoxide Containing Tricyclic Skeleton
Lu Yan ZHANG , Wen Qian YANG , Shi Zhi CHEN , Liang HUANG
1997, 8(1): 15-16
[Abstract](167) [FullText HTML] [PDF 77KB](0)
An unexpected compound,hydroperoxide (4) formed from (3),the exo-cycloaddition product,which was synthesized through the Lewis acid catalyzed intramolecular Diels-Alder (IMDA) reaction.Its structure was confirmed by spectra and X-Ray diffraction analysis;An 1O2 oxidation mechanism was proposed.
An Improved Synthesis of dl-Muscone
Han Song CHEN , Xiu Fang LIU , Han Sheng XU
1997, 8(1): 17-18
[Abstract](183) [FullText HTML] [PDF 81KB](0)
M.Stoll's total synthetic route for dl-muscone was improved. 2.15-Hexadecanedione was synthesized by PTC method.and converted into dehydromuscones through intramolecular aldol reaction by the mixture of zinc chloride and the Grinard reagent of isoamyl bromide used as condensing agent.Catalytic hydrogenation of dehydromuscones gave dl-muscone.
Synthesis of (4R)-α-Terpineol
Wen PEI , Eiji Wada , ShuJi Kanemasa
1997, 8(1): 19-20
[Abstract](178) [FullText HTML] [PDF 54KB](1)
(4R)-α-Terpineol,a natural product,was synthesized enantioselectively by an asymmetrical catalised Diels-Alder reaction from-1-phenylsulfonyl-3-buten-2-one with 2-methyl-1,3-butadiene.
Novel Bis-hydroxymethylation of Imidazole and 2-Methylimidazole
Cheng He ZHOU , Zhi Chang LIU , Ru Gang XIE , Hua Ming ZHAO
1997, 8(1): 21-24
[Abstract](223) [FullText HTML] [PDF 151KB](6)
A novel one-pot synthesis of 4,5-bis(hydroxymethyl) imidazoles 2a-b,new ethers 3a-b and a new type of imidazolophane 4b by the bis-hydroxymethylation of imidazole or 2-methyl imidazole with formaldehyde and potassium hydroxide is reported.The structures of these compounds have been established by MS,1HNMR,IR and elemental analyses.
Studies on Agarofurans Ⅰ. New Synthesis of Nor-Ketoagarofuran and 4-Hydroxydihydroagarofuran
Wu Yan ZHANG , Ji Yu GUO , Xiao Tian LIANG
1997, 8(1): 25-26
[Abstract](170) [FullText HTML] [PDF 89KB](0)
Nor-ketoagarofuran (1),one of the furanoids isolated from agarowood oil,has been synthesized in a preparative scale in high yield from olefin 3 in 3 steps.Reaction of nor-ketoagarofuran (1) with CH3MgI afforded 4-hydroxydihydroagarofuran (2),another naturally occurring tetrahydrofuran derivative.
Studies on the Synthesis of Villosol
Ping XIE , Shu Feng CREN , Xiao Tian LIANG
1997, 8(1): 27-30
[Abstract](164) [FullText HTML] [PDF 165KB](0)
The stereocontrolled synthesis of 2,the structure proposed for villosol,was described.The synthetic work has shown that the proposed structure was incorrect.
High-Yield Synthesis and Extraction of Endohedral Metallofullerenes Dy@C2n
Da Yong SUN , Zi Yang LIU , Xing Hua GUO , Wen Guo XU , Shu Ying LIU
1997, 8(1): 31-34
[Abstract](176) [FullText HTML] [PDF 145KB](0)
The successful encapsulation of dysprosium(Dy) into fullerene cages by activating the Dy2O3 containing graphite rods in situ,"back-burning" carbon-arc evaporation with a high-yield of pyridine extraction technique is reported.
Two New Amides from the Roots of Acorus Tatarinowii Schott
Ming Fu WANG , Ai Na LAO , Hong Cheng WANG
1997, 8(1): 35-36
[Abstract](155) [FullText HTML] [PDF 69KB](0)
Two new amides,tataramide A (1) and tataramide B (2),were isolated from the roots of Acorus tatarinowii Schott.Their structures were determined by spectroscopic methods.
Two New Isopimarane Diterpenes from the Roots of Acorus Tatarinowii Schott
Ming Fu WANG , Ai Na LAO , Hong Cheng WANG , Yasuo Fujimoto
1997, 8(1): 37-38
[Abstract](159) [FullText HTML] [PDF 88KB](0)
Two new isopimarane diterpenes,tatarol (1) and tataroside (2) were isolated from the roots of Acorus tatarinowii Schott.Their structures were identified by spectral methods.
A New C-glycosidic Hydrolysable Tannin from Rhodomyrtus tomentosa
Yan Ze LIU , Ai Jun HOU , Chun Ru JI , Yang Jie WU
1997, 8(1): 39-40
[Abstract](159) [FullText HTML] [PDF 96KB](1)
Tomentosin(1),a new C-glycosidic hydrolysable tannin,was isolated from the leaves of Rhodomyrtus tomentosa.Its structure was determined by chemical method and 1HNMR spectroscopic analysis.
New Chromone Glycosides from Hypericum Japonicum
Qing Li WU , Yong Hong LIAO , Sheng Ping WANG , Li Wei WANG , Yu Xiu FENG , Jun Shan YANG , Pei Gen XIAO , Shao Liang HONG
1997, 8(1): 41-42
[Abstract](169) [FullText HTML] [PDF 90KB](0)
From the aerial part of Hypericum japonicum Thunb.ex Murray,two new chromone glycosides,5,7-Dihydroxy-2-(1-methylpropyl) chromone-8-β-D-glucoside and 5,7-Dihydroxy-2-isopropylchromone-8-β-D-glucoside,were isolated and their structures were determined on basis of spectroscopic evidences.
Artubotryside A and B, Two New Flavonol Glycosides from the Leaves of Artabotrys hexapetalus (Annonaceae)
Tong Mei LI , Jing Guang YU
1997, 8(1): 43-46
[Abstract](168) [FullText HTML] [PDF 170KB](0)
Two new flavonol glycosides,artabotryside A (1),artabotryside B (2),and three known flavonoids taxifolin (3),glucoluteolin (4) and apigenin-7-O-apiosyl (1→2) glucoside(5) were isolated from the leaves of Artabotrys hexapetalus (Annonaceae).The structures of 1 and 2 were established as quercetin-3-O-α-L-rhamnopyranosyl (1→2)-α-L-arabinofuranoside(1) and kaempferol-3-O-α-L-rhamnopyranosyl (1→2)-α-L-arabinofurano-side (2),on the bases of spectral analysis.
The Epimerization of 10-Deacetylbaccatin Ⅲ by Microsphaeropsis Onychiuri a Fungus from Taxus Yunnanensis
Jun Zeng ZHANG , Fu TU , Li He ZHANG , De You QIU
1997, 8(1): 47-48
[Abstract](159) [FullText HTML] [PDF 87KB](0)
The microbiological transformation of a natural taxoid,10-deacetylbaccatin Ⅲ into its C-7 epimer,10-deacetylbaccatin V with Microsphaeropsis onychiuri,a fungus isolated from the inner bark of Taxus yunnanensis is described.
A Possible Multi-stranded DNA Induced by Acid Denaturation-renaturation
Jian Wei LI , Fang TIAN , Chen WANG , Chun Li BAI , En Hua CAO
1997, 8(1): 49-52
[Abstract](162) [FullText HTML] [PDF 156KB](0)
λ-DNA Hind Ⅲ was denatured by HCl,renatured by NaOH,and digested by DNase I sequentially.The produced mixture was separated with Sephadex G200 column,and the chromatograph showed a very weak peak of one component resistant to the digestion of DNase I.The results of AFM studies on this component indicated that an unusual form of DNA was present,with the height 13 times that of double-stranded DNA.By comparison with known results,it is suggested that this is a multi-stranded DNA other than simple supercoils.
RNA Cleavage by N-Phosphoryl Serine in Histidine Buffer
Xiang Hong LI , Yuan MA , Yi CHEN , Yu Fen ZHAO
1997, 8(1): 53-56
[Abstract](154) [FullText HTML] [PDF 470KB](0)
In the presence of histidine.N-(O,O-diisopropyl) phosphoryl serine could catalyze the cleavage of RNA in aqueous solution at neutral pH.The results were detected by sub-marine agarose gel electrophoresis and capillary zone electrophoresis.It was found that at high cpncentration histidine could cleave the RNA slightly.While the participation of DIPP-Ser could significantly accelerate the cleavage reaction.N-phosphodipeptide-N-(O.O-diisopropyl) phosphoryl Ser-His are proposed to be involved in the mechanism.
Application of Rayleigh Light Scattering Spectroscopy to the Determination of Proteins Using Bromo-Pyrogallol Red
Chun Qi MA , Ke An LI , Shen Yang TONG
1997, 8(1): 57-58
[Abstract](167) [FullText HTML] [PDF 77KB](0)
The binding of bromo-pyrogallol red (BPR) to proteins is accompanied by the enhancement of Rayleigh light scattering at 332nm.and based on this.a new quantitative protein assay method is put forward.
Measurement of Ion Mobilities of Selected Amines by Ion Mobility Spectrometry
Yan GUO , Miao Qin LU , Yao Ting LONG
1997, 8(1): 59-60
[Abstract](163) [FullText HTML] [PDF 119KB](0)
The ion mobilities of selected amines were measured by IMS.The minimum detection limits and linear ranges of selected amines were detected.
Adsorptive Stripping Voltammetric Study of the Enhancement of Copper(Ⅱ) in Phosphate and Carbonate media and in the Presence of Silicate
Ming SONG , Hui Min MA , Yue Xian HUANG , Shu Quan LIANG
1997, 8(1): 61-64
[Abstract](155) [FullText HTML] [PDF 169KB](0)
Adsorptive enhancements of several inorganic salts 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 phosphate or carbonate media owing to adsorption.Silicate can also enhance the peak current of Cu(Ⅱ).The enhancing power of phosphate,carbonate,and silicate is 33,26,and 8.9 times,respectively.
Determination of Chromate Ion in Water Using High Performance Capillary Electrophoresis
Qing GUO , Li Wen CHANG , Yu Xian LI , Hai Yu ZHAO
1997, 8(1): 65-66
[Abstract](159) [FullText HTML] [PDF 78KB](0)
A new rapid method for the analysis of chromate ion in water by using high performance capillary electrophoresis is described.The detection limit is 1.0 μg/ml by using 100 m mol/1 Tris-HCl buffer containing 2 m mol/l 1,6-hexanediamine which was used as an electroosmosis modifier to improve the separation and detection sensitivity.
High Performance Hydrophobic Interaction Chromatography-A New Approach to Separate Intermediates of Protein Folding Ⅰ. Separation of Intermediates of Urea-unfolded α-Amylase
Quan BAI , Yin Mao WEI , Ming Hui GENG , Xin Du GENG
1997, 8(1): 67-70
[Abstract](149) [FullText HTML] [PDF 202KB](0)
Based on the different hydrophobicities of the intermediates of proteins,the various conformational intermediates of the refolding of α-amylase originally denatured with 8.0 mol/L urea solution were separated with high performance hydrophobic interaction chromatography (HPHIC).Compared to the separation of the same intermediates with weak anion exchange chromatography and size-exclusion chromatography,the result obtained with HPHIC is the best.It would be expected that HPHIC may be a strongly potential tool to separate intermediates of some proteins which cannot be,or cannot completely be refolded by HPHIC.
Ab Initio Study on the Thermal Isomerization from 1,2-Butadiene to 1,3-Butadiene
Wen Lin FENG , Ming LEI , Yan WANG , Ying QIAN
1997, 8(1): 71-72
[Abstract](149) [FullText HTML] [PDF 96KB](0)
Ab initio UHF/6-31G** method has been employed to study the mechanism of the thermal isomerization from 1,2-butadiene to 1,3-butadiene,The energies were corrected at MP2//6-31G**+ZPE(zero-point energy) level.The results indicate that it is a stepwise reaction via a radical intermediate .The calculated activation barriers are 65.01 and 64.16 kcal./mol.,respectively.
Molecular Weight Characterization of Partially Hydrolyzed Polyacrylamide in the Complex Salts Solution
Mei Ling YE , Dong HAN , Liang He SHI
1997, 8(1): 73-74
[Abstract](144) [FullText HTML] [PDF 80KB](0)
The effects of the nature of salts,salt concentration,pH value,degree of hydrolysis as well as surfactant on molecular size of HPAM were studied.It is found that [η] of HPAM changes with all the above variables,and the molecular weight of HPAM can be obtained through [η] measurement at a specific salts environment in which the [η] is independent of above factors.
The Synthesis, Photoconductivity, Photoinduced Charge Transfer, and Other Properties of HEC-TCNQ
Qi FANG , Hong LEI , Dong XU , Duo Rong YUAN
1997, 8(1): 75-78
[Abstract](176) [FullText HTML] [PDF 174KB](0)
The donor-acceptor complex HEC-TCNQ (HEC=9-hydroxyethylcarbazole;TCNQ=tetracyanoquinodimethane) has been synthesized.Under the illumination of Ar+ laser,the photoinduced charge transfer salt HEC+TCNQ- can be formed with a conductivity of at least one order of magnitude larger than that of HEC-TCNQ.
Green Light-Emitting Organic Electroluminescent Device with a New Fluorescent Dye Dispersed in Poly(N-vinylcarbazole) Emitter Layer
Yong QIU , De Qiang ZHANG , Zhi Liang XIE , Xiao Xuan LIU
1997, 8(1): 79-80
[Abstract](147) [FullText HTML] [PDF 80KB](0)
Double-layer organic electroluminescent devices have been constructed.A new fluorescent dye,9,10-bis(phenylethynyl) anthracence,was chosen as the dopant which was molecularly dispersed in the polymer film,and green light was observed from the device with luminance of 130cd/m2 at 17V.
Preparation and Biological Distribution of New BATOs
Jing Tao WANG , Xiang Yun WANG , Yuan Fang LIU
1997, 8(1): 81-82
[Abstract](137) [FullText HTML] [PDF 110KB](0)
Seven new boronic acid adducts of technetium(Ⅲ) tris(dioxime) (BATO) were prepared and the biodistribution in mice of 99mTc labelled BATOs were determined.The uptake of 1.62% ID in mice heart at 2 min after injection of 99mTcCl(MeCDO)3BMe indicates high myocardial extraction of this BATO.99mTcCl(MeCDO)3BMe shows promise as a myocardial perfusion imaging agent.
XRD & XPS Study on the BaF2 Promoted Sm2O3-LaF3 Catalysts
Ji Zhong LUO , Hui Lin WAN
1997, 8(1): 83-86
[Abstract](151) [FullText HTML] [PDF 189KB](0)
Sm2O3-LaF3 and BaF2 promoted Sm2O3-LaF3 catalysts shown good catalytic performance for the Oxidative Dehydrogenation of Ethane(ODE).XRD and XPS characterizations of the catalysts show the structure defects,which may be produced by the partial exchange of anions and cations,enhance the electron donating ability and increase the surface adsorbed oxygen concentration,thus should be favorable to improve the catalytic activity.However,the higher concentration of surface adsorbed oxygen is unfavorable for the ethene selectivity.
Study on Isoelectric Point of Magnesium Aluminum Hydroxide
Shu Hua HAN , De Jun SUN , Wan Guo HOU , Chun Guang ZHANG , Guo Ting WANG
1997, 8(1): 87-90
[Abstract](137) [FullText HTML] [PDF 128KB](1)
Yoon's equation which predicted point of zero charge of complex oxide should predict the zero point of net charge (ZPNC) of mixture of variable and permanent charge rather than the point of zero charge (PZC) of the variable charge component.The calculated values with modified Yoon's equation agreed with the experimental values.
Determination of the Atomic Weight of Samarium
Tsing Lien CHANG , Guang Sheng QIAO
1997, 8(1): 91-94
[Abstract](159) [FullText HTML] [PDF 159KB](1)
The atomic weight of samarium was redetermined as Ar(Sm)=150.3661(2).Application of substitute calibration using the true isotopic ratio of Eu151/153 results in Ar(Sm)=150.3740(10).A summary is given including the results for other five rare earth elements.
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