1996 Volume 7 Issue 2

α-OXOKETENE CYCLIC DITHIOACETALS CHEMISTRY──REACTION OF α,α-DIOXO(ESTER)KETENE CYCLIC DITHIOACETALS WITH BUTANONE
Zai Ming ZHU , Yong Ting XU , Qun LIU , Jie Han HU
1996, 7(2): 95-98
[Abstract](164) [FullText HTML] [PDF 87KB](0)
Abstract:
Cyclic dithioacetals of α,α-dioxo (ester) ketone 3 were reacted with butanone to afford the Michael adducts 4,catalyzed by metal Na.This process provides a new method for the synthesis of ring-compouds in good yield under mild conditions.
ZEOLITE-CATALYZED FRIEDEL-CRAFTS ACYLATION OF AROMATICS:I.SYNTHESIS OF 4-ACYL ANISOLE WITH A HY CATALYST
Qi Long WANG , Yu Dao MA , Xing Dong JI , Hao YAN , Qin QIU
1996, 7(2): 99-102
[Abstract](160) [FullText HTML] [PDF 137KB](0)
Abstract:
A series of aromatic ketones 4-acyl anisole were synthesized with high yield by using carboxylic acids as acylating agents and a HY zeolite as catalyst.
THE SYNTHESIS OF 4,5-BIS(4'-BROMOBENZYLTHIO)-1,3-DITHIOLE-2-THIONE WITH ONE DIMENSIONAL INTERMOLECULAR INTERACTIONS
Fang QI
1996, 7(2): 103-104
[Abstract](166) [FullText HTML] [PDF 100KB](0)
Abstract:
The title compound BBBT-DTT (C17H12Br2S5,Mr=536.42) has been synthesized and its structure feature has been described.BBBT-DTT is characterized by one dimensional chains formed by S…S (head to head) and Br…Br (tail to tail) intermiolecular interactions.
A NEW APPROACH TO SYNTHESIZING 2-ALKOXYCARBONYL-2-METHYL ETHYL TIN TRICHLORIDES AND THEIR COMPLEXES WITH DBSO AND HMPA
Lai Jin TIAN , Fang Xin FU , Hua De PAN
1996, 7(2): 105-106
[Abstract](251) [FullText HTML] [PDF 80KB](0)
Abstract:
A new approach based on transesterification reaction to synthesizing 2-alkoxycarbonyi-2-methyl ethyl tin trichlorides and their complexes with dibenzylsulfoxide (DBSO) and hexam-ethylphosphoramide (HMPA)was reported.They were characterized by elemental analysis,IR and 1HNMR spectra.The possible mechanism for transesterifications was suggested.
STUDIES ON THE SYNTHESES OF FAVELINES
Gang LIN , Xue Chao WANG , Xin Fu PAN
1996, 7(2): 107-108
[Abstract](303) [FullText HTML] [PDF 81KB](0)
Abstract:
A novel and efficient convergent synthesis of 13-demethyldeoxofaveline,a Key intermediate for deoxofaveline,faveline and faveline methyl ether,was achieved by Wittig reaction and selective oxidation.And a novel sixteen-membered ring compound has been obtained in the meantime.
A CONVERGENT SYNTHESIS OF (E,E,E)-3,7,13-TRIMETHYL-6-(i-PROPENYL)-7,14-DIHYDROXY-2,8,12-TETRADECATRIEN-1-METHYLAL
Yi qian Wan , Jing Yu SU , Qing LIU , Long Mei Zeng
1996, 7(2): 109-110
[Abstract](176) [FullText HTML] [PDF 81KB](0)
Abstract:
Starting from geranial a new synthetic route for compound 6,(E,E,E)-3,7-13-trimethyl-6-(i-propenyl)-7,14-dihydroxyl-2,8,12-tetradecatrien-1-methylal,a key intermediate in the synthesis of diterpene epi-mayol is described.
SYNTHESIS OF ANALOGUES OF HUPERZINE A 4.THE PREPARATION OF A PYRIMIDONE ANALOGUE OF HUPERZINE A
Yun Long LI , Xu Chang HE , Dong Lu BAI
1996, 7(2): 111-114
[Abstract](175) [FullText HTML] [PDF 155KB](0)
Abstract:
The preparation of a pyrimidone analogue 2 of huperzine A is described,in which the pyridone ring of the natural alkaloid is replaced by pyrimidone.The key intermediate β-ketoester 9 was obtained from cyclohexane-1,4-dione monoethylene ketal via 6 steps.Then using the methodology of total synthesis of huperzine A,the construction of bicyclo[3.3.1]nonane moiety substructure was achieved,and 2 was finally afforded in low yield.
SYNTHESIS AND ANTICHOLINERGIC ACTIVITIES OF 6,11-DIHYDRODIBENZ[b,e]OXEPIN AND 6,11-DIHYDRODIBENZO[b,e]THIEPIN HYDROXYCARBOXYLATES
Shou Hai GAO , Liu Hong YUN
1996, 7(2): 115-118
[Abstract](160) [FullText HTML] [PDF 122KB](0)
Abstract:
New tricyclic hydroxycarboxylates-dibenz[b,e]oxepin and dibenzo[b,e]thiepin hydroxycarboxylates (7) were synthesized by modifying the structures of xanthene compounds.The pharmacological results showed the antagonistic activities of these tricyclic compounds were all decreased at different levels after this modification,but they exhibited more selective action on the central nicotinic receptor.Especially,the compounds containing sulfur atom almost have no action on the muscarinic receptors,they were still quite potent to the central nicotinic receptor.
PRACTICAL METHOD FOR SYNTHESIS OF NEW GLYCOLIPIDS N-[4-(DIALKYL-L-GLUTAMATECARBONYLETHYLCARBO-NYLAMINO)BUTYL] LACTOBIONAMIDES
Zhong Zhi ZHANG , Kimitoshi FUKUNAGA , Yoshiaki SUGIMURA , Katsumi NAKAO , Toshimi SHIMIZU
1996, 7(2): 119-122
[Abstract](259) [FullText HTML] [PDF 238KB](0)
Abstract:
A simple and efficient method for the synthesis of new glycolipids containing oligosaccharide and two long alkyl chains N-[4-(dialkyl-L-glutamatecarbony lethylcarbonylamino)butyl]lactobionamide has been developed in moderate yield.We successfully selected succinic anhydride which could condese with dialkyl L-glutamates in almost quantitative yields.The aminolysis of lactonolactone with 1,4-diaminobutane could be carried out in quantitative yield.The glycolipids prepared by this method have three amino acid residues between hydrophobic segment and hydrophilic moiety of the glycolipid which can be considered to maintain the steric conformation of lipase in enzymatic reactions.
POLYCLONAL ANTIBODY-CATALYZED HYDROLYSIS OFβ-NAPHTHOL ACETATE
Bing Hui YANG , Huang Kuan KONG , Ji Qing JIANG , Yong Yong JI , Ming YEH
1996, 7(2): 123-126
[Abstract](162) [FullText HTML] [PDF 137KB](0)
Abstract:
A polyclonal antibody elicited against hapten (4) catalyzed the hydrolysis of β-naphthol acetate with a rate acceleration of 46400 folds.
HYDROLYTIC CLEAVAGE OF ACMET-GLY PROMOTED BY CIS-[Pd(MET)(D2O)2](NO3)2
Xiao Hua CHEN , Long Gen ZHU , N. M. Kostic
1996, 7(2): 127-128
[Abstract](177) [FullText HTML] [PDF 100KB](0)
Abstract:
cis-[Pd(met)(D2O)2]2+ promoted hydrolysis of AcMet-Gly was monitored by 1H NMR spectroscopy.The observed rate constants,koba,strongly depend on the mole ratio of cis-[Pd(met)(D2O)2]2+ to AcMet-Gly.At least,one aqua ligand for each Pd(Ⅱ)is necessary for fast hydrolysis reaction observed.Two aqua ligands of each Pd(Ⅱ) make the reaction faster.
LIPASE-CATAL YZED DOUBLE KINETIC RESOLUTION OF DL-2,4-DIMETHYL-1,5-PENTANEDIOL:A USEFUL SYNTHON IN NATURAL PRODUCT SYNTHESIS
Jian Wen FANG , Zu Yi LI
1996, 7(2): 129-130
[Abstract](179) [FullText HTML] [PDF 94KB](0)
Abstract:
An importment chiral synthon (-)-2,4-dimethyl-1,5-pentanediol and its diester and monoester were obtained by lipase-catalyzed double kinetic resolution.
PREPARATION OF OLIGOSACCHARIDES FROM THE ENZYMATIC HYDROLYSATES OF KONJAC GLUCOMANNAN BY LOW-PRESSURE COLUMN CHROMATOGRAPHY
Gui Yun XU , Li Wen CHANG , Yan Mei XU , Yan He MA , Pei Jin ZHOU
1996, 7(2): 131-132
[Abstract](174) [FullText HTML] [PDF 80KB](0)
Abstract:
Low pressure column chromatography with activated charcoal powder was used to separate the oligosaccharides and their isomers from the hydrolysates of konjac glucomannan.
A NEW DITERPENE FROM SPIRAEA JAPONICA
Xin HONG , Jing Lue NIE , Xiao Jiang HAO
1996, 7(2): 133-134
[Abstract](169) [FullText HTML] [PDF 82KB](1)
Abstract:
Further study on the components of Spiraea japonica var.incisa Yu,resulted in the isolation of a new diterpene spiramilactone,The structure of which was elucidated on the basis of spectral and chemical means.
THE NEW DITERPENE ALKALOIDS FROM ACONITUM TRANSSECTUM
Li Ming GAO , Xiao Jiang HAO , Shang Zheng ZHAN , Xu Wei SHEN , Si Ying CHEN
1996, 7(2): 135-138
[Abstract](239) [FullText HTML] [PDF 128KB](1)
Abstract:
Three new diterpene alkaloids,transconitine A,B and C were isolated from the roots of Aconitum transsectum Diels,and their structures were elucidated by spectral means.
A NEW DITERPENOID ALKALOID FROM DELPHININUM CAERULEUM
Yan WANG , Yuan Jiang PAN , Shao Nong CHEN , Yao Zu CHEN
1996, 7(2): 139-140
[Abstract](160) [FullText HTML] [PDF 79KB](1)
Abstract:
A new minor diterpenoid alkaloid contaning a C(19)-N-azomethine group,caerunine (1) was isolated from Delphinium caeruleum Jacq.ex.Cambss,its struture was determined by spectral data.
NEOLIGNAN GLUCOSIDES FROM PEDICULARIS LONGIFLORA
Chang Zeng WANG , Zhong Jian JIA
1996, 7(2): 141-144
[Abstract](167) [FullText HTML] [PDF 135KB](0)
Abstract:
Two new neolignan glucosides,longiflorosides A and B were isolated from whole plants of Pedicularis longiflora.On the basis of spectral evidence,longiflorosides A and B were determined as (7R,8S)-4-O-methyl-dehydrodiconiferyl alcohol-9'-O-β-D-glucopyranoside and (erythro)-1-(4-O-β-D-glucopyranosyl-3,5-dimethoxy-phenyl)-2-{2-methoxy-4-[1-(E)-propene-3-ol]-phenoxyl}-propane-1,3-diol,respectively.
NEOLIGNAN GLUCOSIDES FROM PEDICULARIS TORTA
Chang Zeng WANG , Zhong Jian JIA
1996, 7(2): 145-148
[Abstract](170) [FullText HTML] [PDF 147KB](0)
Abstract:
Two new neolignan glucosides,tortosides D and E were isolated from plants of Pedicularis toria.On the basis of spectral evidence,tortosides D and E were determined as (7R,8S)-dehydrodiconiferyl-9-O-β-D-4"-O-methyl-glucopyranoside and (7R,8S)-5-methoxy-dihydrodehydrodiconiferyl alcohol-9'-O-β-D-glucopyranoside,respectively.
CYCLOPEPTIDES FROM STELLARIA DELAVAYI
Yu Rut ZHAO , Jun ZHOU , Xiang Kai WANG , Hou Ming WU , Xiao Lin HUANG
1996, 7(2): 149-152
[Abstract](197) [FullText HTML] [PDF 172KB](1)
Abstract:
Further chemical study on Stellaria delavayi led to the isolation of two other new cyclopeptides,namely stelladelin B and C.On the basis of spectroscopic analysis and chemical evidence,their structures were established as cyclo(Gly-Ile-Pro2-Pro1-Ala-Tyr-Asp-Leu) and cylo(Val-Pro3-Tyr2-Pro2-Pro1-Phe-Tyr1-Ser),respectively.
CONFORMATION ANALYSIS OF TUNICAMYCIN V AND ITS NATURAL SUBSTRATE
Min Bo CHEN , Yu LIU , Zhong Wu GUO
1996, 7(2): 153-156
[Abstract](169) [FullText HTML] [PDF 194KB](0)
Abstract:
Conformation analysis of the model compounds for tunicamycin V and its natural donor substrate,UDP-N-acetylglucose,is performed to reveal the detail of the inhibition process.
THEORETICAL STUDIES ON THE INTRINSIC REACTION COORDINATE OF THE REACTION HCO+HNO2→HCHO+NO2
Xian Yong PANG , Yan WANG , Yong Ping YANG , Wen Lin FENG , Shao Wen ZhANG
1996, 7(2): 157-158
[Abstract](180) [FullText HTML] [PDF 79KB](0)
Abstract:
The geometries of the reactants,the transition states(TS) and the products for the reaction HCO+HNO2→HCHO+NO2 have been optimized by using the energy gradient approach at UHF/6-31G level,and the energies were corrected at the MP2/6-31G level.The calculated barrier(48.15KJ·mol-1) for the reaction is in reasonable agreement with the experimental data (28.84±2.51KJ·mol-1).The Intrinsic Reaction Coordinate (IRC) for the reaction is traced by using Morokuma's magnitude method.The variations of the geometries and the potentials for the reaction system are elucidated along the IRC.
HIGH-PERFORMANCE CAPILLARY ELECTROPHORESIS OF REDUCING OLIGOSACCHARIDES AS THEIR ETHYL P-AMINOBENZOATE DERIVATIVES
Li Wen CHANG , Qing GUO , Zhao Lou YU , Yi CHEN , An ZHU
1996, 7(2): 159-160
[Abstract](159) [FullText HTML] [PDF 89KB](0)
Abstract:
A modified method for the separation of oligosaccharides derivatized with p-aminobenzoate ethyl ester by high performance capillary electrophoresis (HPCE) is described.The isomers of larger oligosaccharides up to 10-mers were separated by HPCE with borax as running buffer.
DETERMINATION OF TRACE FLUORIDE AND MOLYBDENUM IN SERUM SAMPLE BY ELECTROCHEMICAL ANALYSIS
Li Zeng WANG , Xiao ZHANG , Yong YU , Cheng Song MA
1996, 7(2): 161-164
[Abstract](163) [FullText HTML] [PDF 139KB](0)
Abstract:
In this paper,the determination of both fluoride and molybdenum can be carried out in the same serum sample as follows:the content of fluoride is determined by direct potentiometry in the solution containing (CH2)6N4 and HNO3 (pH=5.4) while that of molybdenum is determined by adsorptive voltammetry after the above-mentioned solution has been nitrified with mixed acid containing HNO3 and HClO4.
CAN ADSORPTION BE STUDIED IN THE ELECTRODEPOTENTIAL RANGE OF SEVERE HYDROGEN EVOLUTION
Wu Hu Li , Shou Zhong ZOU , Bin REN , Zhong Qun TIAN
1996, 7(2): 165-166
[Abstract](176) [FullText HTML] [PDF 98KB](0)
Abstract:
Surface enhanced Raman spectroscopy (SERS) has been applied to obtain structural information of surface species adsorbed at electrode surface in the electrode potential range of severe hydrogen evolution,which is very difficult to be gained by using most of spectroelectrochemical and conventional electrochemical methods.
FABRICATION OF BIENZYME MALTOSE SENSOR USING MOLECULAR DEPOSITION TECHNIQUE
Chang Qing SUN , Xi ZHANG , Yi Peng SUN , Jia Cong SHEN
1996, 7(2): 167-168
[Abstract](264) [FullText HTML] [PDF 79KB](0)
Abstract:
A new kind of bienzyme maltose sensor was fabricated using molecular deposition technique,in which glucose oxidase and glucoamylase were alternatively deposited with bipolar quaternary ammonium salt on 3-mercapto propionic acid modified gold electrode.Its response performance is described in detail.
OSCILLATION FREQUENCY THEORY OF A PIEZOELECTRIC SENSOR INLIQUID PHASE WITH TWO SEPARATED-ELECTRODES
Da Zhong SHEN , Ze Chang LIU , Qing KANG , Jind Tian HU
1996, 7(2): 169-172
[Abstract](163) [FullText HTML] [PDF 183KB](0)
Abstract:
In this paper,an oscillation frequency equation for a piezoelectric sensor with two separated-electrodes is theoretically derived and experimentally verified.The correlations of the oscillation frequency and the liquid properties are investigated.
PHOTOINDUCED INTRAMOLECULAR CHARGE TRANSFER IN SELF-ASSEMBLY.1.AGGREGATION AND DUAL FLUORESCENCE OF ETHYL P-DIDECYLAMINOBENZOATE IN DIOXANE-WATER BINARY SOLVENT
Yun Bao JIANG
1996, 7(2): 173-176
[Abstract](170) [FullText HTML] [PDF 187KB](0)
Abstract:
Aggregation of ethyl p-didecylaminobenzoate (EDOAB) in dioxane-water binary mixture was shown to occur at water volume fraction of 0.47 and a strong intramolecular charge transfer emission was observed in the aggregate.
ON THE STUDY OF SODIUM-P-NITROPHENOL COMPLEX
Pei Ju SUN , Wen Sheng GUO , Yang LU , Qi Tai ZHENG
1996, 7(2): 177-180
[Abstract](269) [FullText HTML] [PDF 145KB](0)
Abstract:
This paper reports a complex of sodium chloride with p-nitrophenol,which has not previously been published.The composition and formation constant of the complex have been studied by ion-selective electrode,crystal structure of the complex has been measured.
No complexes were formed for lithium and potassium.
CRYSTAL CHEMISTRY STUDY ON PHENOLS PART 2. MOLECULAR PACING ANALYSIS
De Chun ZHANG , Yan Qiu ZHANG
1996, 7(2): 181-184
[Abstract](168) [FullText HTML] [PDF 205KB](0)
Abstract:
Intermolecular Hydrogen Bonding (HB) Patterns in 69 crystal structures of phenols and its simple derivatives were analysed by a non-graphic method automatically.Presented here are the results which are well consistent with the literature reports.
A NEW METHOD FOR PREPARATION OF IRON(Ⅱ) PORPHYRIN COMPLEX-ISOLATION AND CHARACTERIZATION OF AMINE COMPLEX OF FERROUS PORPHYRIN
Xin Hua ZHONG , Yao Yu FENG , Jie Sheng HUANG , Pan Wen SHEN
1996, 7(2): 185-186
[Abstract](164) [FullText HTML] [PDF 94KB](0)
Abstract:
The six-coordinate complex [Fe(Ⅱ)(TPP)(NH2Bu1)2] (TPP=mesotetraphenylporphyrinate) has been prepared by i-butylamine reduction method in the existence of antiformin in aerobic solution.The complex was characterized by UV-Vis spectroscopy,IR spectroscopy and elemental analysis.
A NEW METHOD FOR PREPARATION OF IRON(Ⅲ) PORPHYRIN OXYANION COMPLEXES-SYNTHESIS OF PERCHLORATE(PORPHYINATO) IRON(Ⅲ)
Xin Hua ZHONG , Yao Yu FENG , Jie Sheng HUANG , Pan Wen SHEN
1996, 7(2): 187-188
[Abstract](164) [FullText HTML] [PDF 71KB](0)
Abstract:
A new method for preparation of iron(Ⅲ) porphyrin oxyanion complexes was reported.By this method perchlorate complex of iron(Ⅲ) tetraphenylporphyrin [FeTTP(OClO3)] was prepared from i-butylamine complex of iron(Ⅱ) porphyrin [Fe(TPP(NH2Bui)2 by treatment with perchloric acid.
PREPARATION OF HETEROBIMETALLIC COMPLEXES BRIDGING WITH π,π-BOUND PHENYLCYCLOPENTADIENYL LIGAND AND X-RAY CRYSTAL STRUCTURE OF (TRICARBONYL-π-CHROMIUM)PHENYLCYCLOPENTADIENYLCOBALT DICARBONYL
Chang Tao QIAN , Jian Hua GVO , Jie SUN
1996, 7(2): 189-192
[Abstract](164) [FullText HTML] [PDF 155KB](0)
Abstract:
(Tricarbonyl-π-chromiurn)phenylcyclopentadienyl transition metal (Ti,Mo,Mn,Ru,Co) complexes have been synthesized.The crystal structure of (tricarbonyl-π-chromium)phenylcyclopentadienylcobalt dicarbonyl (3) was determined by X-ray diffraction:crystals are orthorhombic.space group P212121,a=15.083(5),b=16.391(5),c=6.351(4) A,V=1570(1) A3 and Z=4.The phenyl ring and the cyclopentadienyl ring in the molecule are not coplanar (dihedral angle:25°).
PREPARATION AND CHARACTERIZATON OF MICROPOROUS CATALYTIC MATERIALS WITH NARROW PORE DISTRIBUTION AND HIGHLY DISPERSED PALLADIUM
An Wu Li , Guo Xing XIONG , Hong Bin ZHAO , Jing Hua Gu , Shi Shan SHENG , Wei CUI , Lu Bin ZHENG
1996, 7(2): 193-194
[Abstract](160) [FullText HTML] [PDF 109KB](0)
Abstract:
The catalyst Pd/γ-Al2O3 was prepared by modification of γ-AlOOH sol particles with the complex of palladium salt with sol-gel technique in this letter.The pore distribution of the support γ-Al2O3 was very narrow from nitrogen adsorption measurement and the palladium in the γ-Al2O3 was highly dispersed determined from hydrogen chemisorption experiment.
THERMOSTABILITY OF LiCu2O2 AND LiCu3O3
Jian Hua LIN , Kai LI , Shen Kang RUAN , Miau Zeng SU , Eberhard SCHWEDA
1996, 7(2): 195-198
[Abstract](284) [FullText HTML] [PDF 194KB](6)
Abstract:
Thermostability and phase transformation of LiCu2O2,LiCu3O3 and other related copper oxides have been studied by x-ray powder diffraction technique at high temperature in air.Both LiCu2O2 and LiCu3O3 are metastable at room temperature.LiCu2O2 decomposes to Li2CuO2 and a monoclinic phase with CuO structure,while LiCu3O3 transforms to the monoclinic phase at lower temperature.Moreover,evidence for a possible intermediate phase between LiCu3O3 and Li0.25Cu0.75O0.85 has also been presented.
PREPARATION AND CHARACTERIZATION OF NIOBIUM-CONTAINING DIMOLYBDO-15-TUNGSTODIPHOS-PHORIC SALT
Jian GONG , Lun Yu QU
1996, 7(2): 199-200
[Abstract](167) [FullText HTML] [PDF 77KB](0)
Abstract:
Preparation of P2W15Mo2NbO627- was reported in the paper.It was characterized by elementry analysis,IR,UV,polarography,183W-NMR and XPD spectra.All results showed the structure of the heteropoly anion was the Dawson type.
ON SIMULTANEOUS SUBSTITUTION OF TI AND V INTO MCM-41 TYPE MOLECULAR SIEVE
Zhong Yong YUAN , Jing Zhong WANG , He Xuan LI
1996, 7(2): 201-204
[Abstract](162) [FullText HTML] [PDF 193KB](0)
Abstract:
The new crystalline V-Ti-silicalite with mesoporous MCM-41 type molecular sieve structure is synthesized hydrothermally;The framework IR spectra associated with ESR,29Si MAS NMR,DRS and XPS data shows that V and Ti are simultaneously incorporated into V-TiMCM-41 framework.
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