2001 Volume 12 Issue 4

CO2 Adducts of the Amino and Imino Groups Studied by 1HNMR and 13CNMR
Zhen CHEN , Ren Yun WANG , Li Lian ZHU , Xiao Tian LIANG
2001, 12(4): 283-286
[Abstract](155) [FullText HTML] [PDF 30KB](0)
CO2 adducts of L-(+)-asparaginic acid and some polyhydroxylated alkaloids was studied by 1HNMR and 13CNMR in this paper.
Dehalogenation of Aryl Halides Catalyzed by MontK10 Immobilized PVP-Pd-Sn Catalyst in Aqueous System
Xiao Li ZHEN , Jian Rong HAN , Ru Hong KANG , Xing Mei OUYANG
2001, 12(4): 287-290
[Abstract](147) [FullText HTML] [PDF 23KB](1)
A series of PVP-Pd-Sn/MontK10 catalysts were prepared by immobilization of PVP [poly (N-vinyl-2-pyrrolidone)] supported bimetallic catalyst using MontK10 as carrier. This catalyst has good catalytic activity for hydrogen transfer dehalogenation of aryl halides. The catalytic reaction was carried out in aqueous system in the presence of phase transfer catalyst and sodium formate as hydrogen source. The catalyst with loading Pd 0.19wt% and molar ratio of Pd/Sn 8:1 gives the highest activity and good stability. This catalyst is more reducible with NaBH4. It is also found that the catalyst is easily separated from the reaction system.
Baker's Yeast Mediated Reduction of Optically Active Diketone
Xiao Lei GAO , Gang ZHOU , Yu Kun GUAN , Wei Dong LI , Yu Lin LI
2001, 12(4): 291-292
[Abstract](151) [FullText HTML] [PDF 22KB](0)
Baker's Yeast mediated reduction of optically active diketone has been described.
Studies on New Additions to 5-Methoxy-2 (5H)-Furanone:1, 4-Addition of Grignard Reagents, and 1,3-Dipolar Cycloaddition of Silyl Nitronates
Zhao Yang WANG , Jia Ling CUI , Bao Shan DU , Qing Hua CHEN
2001, 12(4): 293-296
[Abstract](160) [FullText HTML] [PDF 27KB](1)
1,4-Addition reaction of Grignard's reagent to 5-methoxy-2 (5H)-furanone 1 was accomplished, which provided a new possible route for synthesizing β-alkyl-γ-alkyloxy-γ-butyrolactone. A novel concise method of preparing fused heterocyclic compounds was offered by 1,3-dipolar cycloaddition reaction of silyl nitronates to 1.
Synthesis of Novel Diterpenequinone Salvicine from Ferruginol
Xin CHEN , Jin Sheng ZHANG , Ming ZHAO
2001, 12(4): 297-300
[Abstract](158) [FullText HTML] [PDF 25KB](0)
An efficient synthetic route has developed to the antitumor compound salvicine via 9 steps from ferruginol. The key reaction is the rearrangement of the angular methyl group of compound 7 to 4,5-seco-5,10,-friedo-abieta diterpene 8.
A Novel Synthesis of Some Hexasubstituted Cyclotriphosphazenes
Cheng Feng YE , Ze Fu ZHANG , Wei Min LIU
2001, 12(4): 301-304
[Abstract](158) [FullText HTML] [PDF 26KB](0)
Some known and new hexaaryloxyphosphazene N3P3 (O-C6H4-R)6] (R=H, CH3, OCH3, C(CH3)3, CHO, F, C6H5COOR, etc) were readily obtained with ca. 70% isolated yield in refluxing acetonitrile in the presence of anhydrous potassium phosphate. All compounds were characterized by means of elemental analysis,1H-NMR,31P-NMR spectroscopy.
Lipase-catalyzed hydrolysis of methyl-3-phenylglycidate
Guo Jun ZHENG , Jian Jun WANG , Tian Rui REN , Liu YANG , Wan Ru SUN
2001, 12(4): 305-306
[Abstract](144) [FullText HTML] [PDF 19KB](0)
The enzymatic resolution of racemic methyl 3-phenylglycidate was investigated. It was found that the hydrolysis rate of (2S, 3R)-enantiomer was faster than that of (2R, 3S)-enantiomer by a new lipase. At optimal condition 96% of (2R, 3S)-methyl phenylglycidate with ee of 100% was recovered from the racemic mixture.
Photochemical Reduction of Aromatic Imines by 2-Phenyl-N, N-dimethylbenzimidazoline
Mei Zhong JIN , Li YANG , Long Ming WU , You Chen LIU , Zhong Li LIU
2001, 12(4): 307-308
[Abstract](164) [FullText HTML] [PDF 20KB](0)
A series of aromatic imines were reduced to corresponding amines in excellent yields by 2-phenyl-N, N-dimethylbenzimidazoline (PDMBI) photochemically in the presence of magnesium perchloride (Mg(ClO4)2). A Mg2+ mediated photoinduced electron transfer mechanism was proposed.
Effect of Reaction Media on Photoreaction of Provitamin D3
Yun Yan GAO , Yong Yong LIU , Bo Jie WANG , Bao Wen ZHANG , Yi LI
2001, 12(4): 309-312
[Abstract](157) [FullText HTML] [PDF 26KB](0)
The photoisomerization of provitamin D3 is carried out in silica gel-hexane matrix, ethanol and hexane. The results show that in silica gel-hexane matrix and ethanol, the desired product of prevtamin D3 and vitamin D3 can be obtained in high yield, while the undesirable byproducts are greatly limited.
Oligouridylates Formation with N-(O,O'-Diisopropyl)-Phosphoryl Alanine in the presence of Poly (β-(N7-Adeninyl) Ethyl Methacrylate)
Hong Qi XIANG , Jian Jun HU , Yang JIANG , Yu Fen ZHAO
2001, 12(4): 313-316
[Abstract](153) [FullText HTML] [PDF 33KB](0)
The oligouridylates formation with N-(O,O-diisopropyl)-phosphoryl alanine in the presence of poly(β-(N7-adeninyl)ethyl methacrylate) was studied. An increased yield by the presence of the polymeric nucleic acid analog was confirmed by anion exchange column HPLC, C18 reverse phase HPLC, and turbo ionspray MS.
Study on the Structure of Supramolecular Inclusion Complex of β-Cyclodextrin with Retinoic Acid
Yan Ling ZHANG , Wei Sheng LIU , Yang LI , Xue Yi MA , Yao Zu CHEN
2001, 12(4): 317-320
[Abstract](150) [FullText HTML] [PDF 63KB](0)
Inclusion compound of retinoic acid with β-cyclodextrin was prepared by coprecipitating method, the structure of resulting product was studied by elemental analysis, differential scanning caloriemetry (DSC) analysis, FT-IR spectroscopy and X-ray diffractometry, and the formed supramolecule self-assembles in aqueous solution according to molar ratio 2:1 of host-guest.
The Microwave-assisted Preparation and X-Ray Structure of 3-Bromocarbazole-N-Acetic Acid
Wen Jian LAO , Yu Hua ZHANG , Yue Qi LIU , Qiang Jin WU , Zi Xiang HUANG , Qing Yu OU
2001, 12(4): 321-324
[Abstract](144) [FullText HTML] [PDF 74KB](0)
The rapid synthesis of 3-bromocarbazole-N-acetic acid was performed using microwave irradiation. Under the optimal conditions the yield was 85.6%. The crystal structure showed that the carboxylic groups form bifurcated hydrogen bonds and the hydroxyl oxygen atoms serve as proton donors and also acceptor. Each carboxylic group was involved in four hydrogen bonds. The packing of crystal was dominated by links of these hydrogen bonds.
Synthesis and Characterization of Soluble Reactive Copoly (aryl ether ketone ketone)
Yan GAO , Xi Gao JIAN , Zhi Yong XU , Yue GAO , Qian Jiang LÜ
2001, 12(4): 325-326
[Abstract](149) [FullText HTML] [PDF 20KB](0)
Soluble reactive copoly (aryl ether ketone ketone) was synthesized from the condensation of 2,2',3,3',6,6'-hexaphenyl-4,4'-diphenol, 2,2-p-hydroxyphenyl-iso-propane, and 1-methyl-cyclohex-1-ene-4,5-diyl-bis (4-fluorophenyl methanone). FT-IR, DSC and TGA were used to characterize the novel polymer.
Structural Revision of Isovalertatins D03 and D23 Isolated from the Culture Filtrate of Streptomyces luteogriseus
Duan Yun SI , Da Fang ZHONG , Wen Yi HE , Li Mei ZHAO
2001, 12(4): 327-330
[Abstract](150) [FullText HTML] [PDF 79KB](0)
Two aminooligosaccharides, isovalertatins D03 (1) and D23 (2), were isolated from the culture filtrate of Streptomyces luteogriseus. Their structures were reinvestigated and revised by spectroscopic evidences including ESI multistage mass spectrometry and 2-dimensional NMR techniques.
Saikosaponin v-2 from Bupleurum chinense
Hong LIANG , Yan Jun CUI , Yu Ying ZHAO , Bin WANG , Wen Xiu YANG , Yi YU
2001, 12(4): 331-332
[Abstract](157) [FullText HTML] [PDF 26KB](1)
Saikosaponin v-2 (1), was isolated from the roots of the title plant and the structure was identified on the basis of spectral analysis. Saikosaponin v-2 is a new compound, which was identified as 3β,16α,23,28-tetrahydroxy-olean-11,13 (18)-dien-30-oic acid-3-O-β-D-glucopyrano-syl-(1→2) glucopyranosyl-(1→3)-β-D-fucopyranosyl-30-O-xylitol ester.
Two New Compounds from Melanosciadum pimpinelloideum H. Boiss
Yi ZHOU , Guo Lin ZHANG , Bo Gang LI , Yao Zu CHEN
2001, 12(4): 333-334
[Abstract](156) [FullText HTML] [PDF 27KB](2)
Two new compounds, melanochromone and 2-ethoxyl-2-(4-hydroxyphenyl) ethanol, were isolated from the whole plants of Melanosoiadum pimpinelloideum H. Boiss. The known compounds isolated were 1-(4-hydroxyphenyl)-1,2-ethanediol, tymine, cimifugin, umtatin, bergenin, daucosterol and stigmasterol. Their structures were determined on the basis of spectral data.
A New p-Terphenyl Derivative from Basidiomycetes Boletopsis grisea
Lin HU , Ze Jun DON , Ji Kai LIU
2001, 12(4): 335-336
[Abstract](153) [FullText HTML] [PDF 22KB](0)
A new p-terphenyl derivative 1 was isolated from the fruiting bodies of Boletopsis grisea. Its structure was established as 2, 3-diacetoxy-4', 4'', 5, 6-tetrahydroxy-p-terphenyl by spectroscopic and chemical means.
A New Quinolizidine Alkaloid from Boehmeria siamensis
Ying Gang LUO , Bo Gang LI , Guo Lin ZHANG
2001, 12(4): 337-338
[Abstract](153) [FullText HTML] [PDF 26KB](0)
A new quinolizidine alkaloid, 3-(4-hydroxyphenyl)-4-(3-methoxy-4-hydroxyphenyl)-3, 4-dehydroquinolizidine (1), was isolated from the ethanol extract of the whole plants of Boehmeria siamensis Craib. Its structure was elucidated on the analysis of 1D NMR and 2D NMR spectrum.
The Diterpenoid Quinones from Coleus forskohlii
Chun Suo YAO , Yun Long XU
2001, 12(4): 339-342
[Abstract](148) [FullText HTML] [PDF 31KB](0)
Two new diterpenoid quinones, coleon S and T were isolated from the chloroform extract of the leaves of Coleus forskohlii, and based on spectroscopic data, their structures were identified as 1,4-phenathrenedione-4b,5,6,8a,9,10-hexahydro-3,9b,10a-trihydroxy-4b,7,8-rimethyl-2-(2-ethoxypropyl) (1) and 1,4-phenathrenedione-2,3,4b,5,6, 8a,9,10-octahydro-3,9β,10α-tri-hydroxy-4b,7,8-trimethyl-2-propylene(2), respectively.
A New Monoterpene Glucoside from the Leaves of Betula platyphylla Suk.
Su Juan WANG , Yue Hu PEI , Hui Ming HUA
2001, 12(4): 343-344
[Abstract](146) [FullText HTML] [PDF 22KB](0)
A new monoterpene glucoside, (2E,6Z)-2,6-dimethyl-8-β-D-glucosyloxy-2,6-octadien-oic acid, was isolated from the leaves of Betula platyphylla Suk. The structure was established by spectroscopic data.
A New 24, 30-Dinortriterpenoid from Paeonia delavayi
Shao Hua WU , Xiao Dong LUO , Yun Bao MA , Xiao Jiang HAO , Da Gang WU
2001, 12(4): 345-346
[Abstract](165) [FullText HTML] [PDF 24KB](0)
A new triterpenoid, 3β, 4β, 23-trihydroxy-24, 30-dinorolean-12, 20 (29)-dien-28-oic acid, together with five known compounds, 2α, 3β, 23-trihydroxy-12-oleanen-28-oic acid-b-D-glucopyranosyl ester, palbinone, 2-hydroxy-benzoic acid, vanillic acid, syringic acid, were isolated from the roots of Paeonia delavayi Franch. Their structures were characterized by spectral analysis.
DFT Calculations for Electron Transfer Bond-breaking Reaction of CH3-X
Yu Mei XING , Zheng Yu ZHOU , Ben Ni DU
2001, 12(4): 347-350
[Abstract](150) [FullText HTML] [PDF 59KB](0)
DFT/6-311+g** level calculations are performed to study the electron transfer bond-breaking reaction of CH3-X. The calculated values are in good agreement with the experimental results or the empirical model. Through analyzing the change of the energy and the charge density along the reaction path, the bond-breaking in ET reaction for CH3X is investigated.
Cosolvent Effect on the Tautomerism of Ethyl Acetoacetate in Supercritical CO2
Hong Ping LI , Hai Fei ZHANG , Jun LIU , Bu Xing HAN
2001, 12(4): 351-352
[Abstract](155) [FullText HTML] [PDF 19KB](1)
The effect of cosolvent cyclohexane, chloroform, and acetonitrile on the keto-enol tautomeric equilibrium of ethyl acetoacetate in supercritical CO2 was studied by UV-Vis spectroscopy over the pressure range from 76 to 110 bar at 308.15 K. It was found that the equilibrium constant decreases with increasing polarity of the cosolvents.
Solid State NMR Study of Polystyrene Nanolatex Particles(I) 13C Spin-Lattice Relaxation Time
Ya Lin TANG , Xiao Zhong QU , Liu Sheng CHEN , Xi Gao JIN
2001, 12(4): 353-354
[Abstract](147) [FullText HTML] [PDF 19KB](0)
13C spin-lattice relaxtion times for polystyrene nanolatex particles have been investigated. It was found that the dramatic increase at 80℃ annealing temperature is well below the Tg temperature of bulk polystyrene, the increase of relaxation time of aromatic carbons is larger than that of for aliphatic carbons at transition annealing temperature.
Enantiomeric Separation of Amino Alcohols by Ion-pair Chromatography
Ming Hua HU , Xiu Zhu XU
2001, 12(4): 355-356
[Abstract](154) [FullText HTML] [PDF 23KB](0)
Enantiomers of four amino alcohols were resolved by ion-pair chromatography with (+)-10-camphorsulphonic acid as chiral counter ion. Studies of the influence of the mobile phase composition, the solute structure and the mobile phase flow-rate on separation are presented. Under the optimized conditions, enantiomeric propranolol, norephedrine, metropolol and salbutamol were separated using dichloromethane-1-pentanol (97:3, v/v) as mobile phase on Lichrospher-100-DIOL column.
Determination of Enantiomeric Purity of n-Pyrrolidinyl Phenylpropanol by Capillary Electrophoresis Using β-Cyclodextrin Polymer as Chiral Selector
Tong WU , Xin ZHOU , Jia Hua CHEN , Jun Ling GU , Ruo Nong FU
2001, 12(4): 357-358
[Abstract](168) [FullText HTML] [PDF 19KB](0)
Enantiomer of n-pyrrolidinyl phenylpropanol was studied by capillary electrophoresis using β-cyclodextrin polymer as chiral selector. We determined the enantiomeric excess value of n-pyrrolidinyl phenylpropanol with RSD 0.48%.
Studies on The Adsorption Capacity for Bilirubin of The Adsorbent Chitosan-β-Cyclodextrin
Wei Liang XU , Chun Ling FU , Jun LI
2001, 12(4): 359-362
[Abstract](158) [FullText HTML] [PDF 44KB](0)
The adsorbent crosslinked chitosan-β-cyclodextrin (β-CD) was prepared by the reaction of glutaraldehyde with chitosan and β-cyclodextrin. This type of adsorbent has high adsorption capacity for unconjugated bilirubin. The adsorption capacity was related to the β-CD content of the adsorbent; phosphate buffer concentration; temperature; pH value; ionic strength and the adsorbent beads. The results indicated that the chitosan-β-CD was a good adsorbent for unconjugated bilirubin with high capacity.
Study of Oxidation of Glutathione by Capillary Electrophoresis
Xian LUO , Jian De LU , Xiao Yun FU
2001, 12(4): 363-364
[Abstract](154) [FullText HTML] [PDF 25KB](0)
A capillary electrophoresis method for the separation and quantification of reduced glutathione (GSH) and oxidized glutathione (GSSG) was developed. A baseline separation was achieved within five minutes. The effects of time and the concentrations of hydrogen peroxide (H2O2) on the oxidation of GSH were investigated.
Deconvolution Method for Determination of the Nitrogen Content in Cellulose Carbamates
Guang Mei CHEN , Yi Ping HUANG
2001, 12(4): 365-368
[Abstract](172) [FullText HTML] [PDF 52KB](4)
Cellulose carbamates (CC) were synthesized with microcrystalline cellulose as raw materials. The Fourier transform infrared spectra of CC with different nitrogen content were recorded. The accurate results of the nitrogen content for CC can be obtained by using the deconvolution method when the nitrogen content is less than 3.5%. The relationship between the nitrogen content and the absorption intensity ratio of the corresponding separated absorption peaks in FTIR spectra has been expressed by an equation precisely.
Fluorescence Spectra of Model Compounds for Light-emitting Alternating Copolymers in Heterogeneous Environments
Jun Lin YANG , Hong Zhen LIN , Min ZHENG , Feng Lian BAI
2001, 12(4): 369-372
[Abstract](161) [FullText HTML] [PDF 44KB](0)
In this paper, the fluorescence spectra of model compounds of light-emitting alternating copolymers, M (TPA-PPV) and M (TPA-PAV) (Scheme 1) were studied and the effect of KNO3 on the interaction between model compounds and ionic micelle-water interface was also investigated. It is found that (I) The fluorescence changes of M (TPA-PPV) are related to the state of CTAB and SDS solution. (Ⅱ) Aggregated state can be formed in M (TPA-PAV) solution at low concentration of CTAB. (Ⅲ) Higher concentration of KNO3 may affect the interaction between model compounds and ionic micelle-water interface.
A New Organo-Directed Titanium Phosphate Phase Containing Zigzag Chains of Corner-Sharing TiO6 Octahedra
Yang Hong GUO , Zhan SHI , Ding HONG , Ya Bo WEI , Wen Qin PANG
2001, 12(4): 373-376
[Abstract](159) [FullText HTML] [PDF 0KB](0)
A new organo-directed titanium phosphate,[NH3CH2CH2NH3]·[TiO(HPO4)2], was synthesized by the solvothermal method and its structure was determined by single crystal X-ray diffraction. The structure consists of 1-D zigzag chains built up from trans-corner-sharing titanium oxo octahedra running along the b axis, with fused Ti2P three-membered rings being attached to the-Ti-O-Ti-O-backbone.
A New Organo-Directed Titanium Phosphate Phase Containing Zigzag Chains of Corner-Sharing TiO6 Octahedra
Yang Hong GUO , Zhan SHI , Ding HONG , Ya Bo WEI , Wen Qin PANG
2001, 12(4): 373-376
[Abstract](132) [FullText HTML] [PDF 64KB](0)
A new organo-directed titanium phosphate,[NH3CH2CH2NH3]·[TiO(HPO4)2], was synthesized by the solvothermal method and its structure was determined by single crystal X-ray diffraction. The structure consists of 1-D zigzag chains built up from trans-corner-sharing titanium oxo octahedra running along the b axis, with fused Ti2P three-membered rings being attached to the-Ti-O-Ti-O-backbone.
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