2001 Volume 12 Issue 5

Reaction of Arylselenium Titanocene Complexes with Diaryl Iodonium Salts——a Convenient Synthesis of Unsymmetrical Diarylselenides
Xiang HUANG , Lu Ling WU , Xin Hua XU
2001, 12(5): 377-378
[Abstract](449) [FullText HTML] [PDF 21KB](0)
Abstract:
The diaryldiselenides reacted with titanocene hydried (Cp2TiH) generted from Cp2TiCl2/i-BuMgBr to give arylselenium complexes of titanocene.They reacted readily with diaryliodoiums salt to give unsymmetical diarylselenides.
Reduction of Elemental Selenium by Samarium Diiodide:the Synthesis of Dithiodiselenides and Dithioselenides
Hong Yun GUO , Yun Fa ZHENG , Yong Min ZHANG
2001, 12(5): 379-382
[Abstract](447) [FullText HTML] [PDF 29KB](2)
Abstract:
The reduction of elemental selenium by samarium diiodide led to selective formation of selenolate anion species (Se22- and Se2-),these nucleophilic species reacted readly with sodium alkyl thiosulfates to afford dithiodiselenides and dithioselenides in moderate to good yield under mild conditions.
A Rapid and Efficient Synthesis of Diaryl Thioureas via Solvent-Free Reaction Using Microwave
Jian Ping LI , Qian Fu LUO , Yu Min SONG , Yu Lu WANG
2001, 12(5): 383-386
[Abstract](459) [FullText HTML] [PDF 26KB](1)
Abstract:
A rapid and efficient method for the preparation of diaryl thiourea compounds was reported for the first time.Twelve diaryl thiourea compounds that possessing biological activity have been synthesized in excellent yields (91-97%).The reaction proved to be extremely simple and highly efficient (in 1.5-4.5 min).
A One-pot Procedure to Prepare Ethynylferrocene and Iodoethynylferrocene
Ji Shan WU , Chun Yan CHI , Xian Hong WANG , Xiao Jiang ZHAO , Ji LI , Fo Song WANG
2001, 12(5): 387-390
[Abstract](443) [FullText HTML] [PDF 28KB](2)
Abstract:
Ethynylferrocene and iodoethynylferrocene were prepared in high yield as 88-90% through a one-pot procedure.1,1'-diiodoferrocenylene was in-situ prepared from reaction of CHI3 PPh3,t-BuOK and ferrocenecarboxaldehyde,further reaction with t-BuOK or n-BuLi gave the title compounds.
Coupling Reaction of 4-Chloro-7-H-Pyrrolo [2,3-d]Pyrimidine with 2,3,5-Tri-O-Acetyl-β-D-Ribofuranosyl Chloride
Yun Long ZHANG , Liang Ren ZHANG , Zhen Jun YANG , Ji Mei MIN , Li He ZHANG , Yang LU , Ning Bo GONG , Qi Tai ZHENG
2001, 12(5): 391-394
[Abstract](466) [FullText HTML] [PDF 44KB](0)
Abstract:
Coupling reaction of 4-chloro-7-H-pyrrolo [2,3-d]pyrimidine with 2,3,5-tri-O-acetyl-β-D-ribofuranosyl chloride under the basic condition was investigated.An abnormal coupling reaction,in which the heterocyclic base attacked at the carbon of 1,2-O-methylidene moiety instead of anomeric carbon of ribose was observed and the structure of products 5a,5b were identified by NMR and X-Ray diffraction.
The Enantioselective Addition of Diethylzinc to Aldehydes Catalyzed by 2-Methylquinoline Derived Chiral Ligands
Qian Yong XU , Guo Xing WANG , Xin Fu PAN
2001, 12(5): 395-396
[Abstract](454) [FullText HTML] [PDF 22KB](0)
Abstract:
Readily available 2-methylquinoline derived chiral ligands 1 and 2 have been applied in the enantioselective addition of diethylzinc to aldehydes with up to 91.4% ee being recorded.
Stereoselective Functionalization at C-2 and C-3 of the Gibberellin via an Intramolecular Free Radical Cyclization Approach
An Qi CHEN , Christine L. WILLIS
2001, 12(5): 397-398
[Abstract](454) [FullText HTML] [PDF 25KB](0)
Abstract:
Stereoselective functionalization at C-2 and C-3 of the gibberellin skeleton was achieved via an intramolecular free radical cyclization approach using a tethered C-19 halomethyl ester as the radical precursor.
A Novel Palladium-Catalyzed Reaction and Its Application in Preparation of Derivatives of Stilbazols
Zhi Yong WANG , Chao JIANG , Ji Hui WU , Qing Xiang GUO
2001, 12(5): 399-402
[Abstract](459) [FullText HTML] [PDF 34KB](3)
Abstract:
A novel palladium-catalyzed coupling reaction for the preparation of derivatives of stilbazoles was presented.A series of stilbazoles were synthesized firstly by this highly efficient method.From this reaction it was found that reaction solvent is one of important factors in this catalytic system.
Diastereoselective Michael Addition of (4'S)-Ethyl-3-(2',2'-Dimethyl-1',3'-dioxolan-4'-yl) acrylate with Furyl Lithium
Dong Mei HAN , Xun Tian JIANG , Jian Hong CHEN , Bin WANG , Dong Lu BAI
2001, 12(5): 403-406
[Abstract](450) [FullText HTML] [PDF 38KB](0)
Abstract:
Michael addition of the chiral α,β-unsaturated ester 2 with furyl lithium proceeded in syn manner with excellent diastereoselectivity.The diastereoselectivity was not affected by the configuration of the double bond in 2.
First Total Synthesis of 5α-Hydroxy-isopterocarpolone
Gang ZHOU , Xiao Lei GAO , Yu Kun GUAN , Wei Dong LI , Yu Lin LI
2001, 12(5): 407-408
[Abstract](448) [FullText HTML] [PDF 26KB](0)
Abstract:
The first total synthesis of 5α-hydroxy-isopterocarpolone has been described.
First Total Synthesis of 7-O-Geranyl-pseudobaptigenin
Ya Ping WANG , Liang Xi LI , Jian Jun CHEN , Qing Lian WANG , Yu Lin LI
2001, 12(5): 409-410
[Abstract](447) [FullText HTML] [PDF 24KB](0)
Abstract:
Total synthesis of 7-O-geranyl-pseudobaptigenin is described,the key steps are Grignard reaction and cyclization reaction.
Synthesis and Characterization of the Terpolymer of Itaconic Acid with Acrylamide and 2-Acrylamido-2-methylpropanesulfonic Acid
Yu Min WU , De Jun SUN , Tao WU , Chun Guang ZHANG
2001, 12(5): 411-412
[Abstract](451) [FullText HTML] [PDF 27KB](2)
Abstract:
The terpolymer of itaconic acid,acrylamide and 2-acrylamido-2-methyl-1-propane sulfonic acid was synthesized through the free-radical polymerization.The IR spectra confirmed that there was no olefinic band,while the TGA results revealed that the terpolymer was of high thermal stability.
Design and Synthesis of Chiral Molecular Tweezers Based on Deoxycholic Acid
Cui Hua XUE , Qi Ming MU , Shu Hua CHEN
2001, 12(5): 413-416
[Abstract](449) [FullText HTML] [PDF 36KB](0)
Abstract:
A series of new chiral molecular tweezers have been designed and synthesized by using deoxycholic acid as spacer and aromatic amines as arms.Instead of using toxic phosgene,the triphosgene was employed in synthesis of the molecular tweezers receptors.These chiral molecular tweezers showed good enantioselectivity for D-amino acid methyl esters.
Synthesis and Characterization of (E)-5-[2-(N-hexylcarbazolyl) vinyl] furan Derivatives with Acceptor Groups
Jian Li HUA , Wei ZHANG , Jing Dong LUO , Jin Gui QIN
2001, 12(5): 417-318
[Abstract](445) [FullText HTML] [PDF 20KB](1)
Abstract:
A new series of (E)-5-[2-(N-hexylcarbazolyl) vinyl] furan chromophores with various acceptors have been synthesized by the Knoevenagel condensation of (E)-5-[2-(N-hexylcarbazolyl) vinyl]-2-furaldehydes with malononitrile,1,3-diethyl-2-thiobarbituric acid,or 3-phenyl-5-isoxazol one,respectively.They are characterized by 1H-NMR,FT-IR,UV-VIS,MS and elemental analysis,and have shown strong solvatochromism and high thermal stability.
Synthesis of Pyridazinonethiadiazoles as Possible Antifungal Agents
Xia Juan ZOU , Gui Yu JIN
2001, 12(5): 419-420
[Abstract](459) [FullText HTML] [PDF 22KB](0)
Abstract:
Several 5-[1-aryl-1,4-dihydro-6-methylpyridazin-4-one-3-yl]-2-arylamino-1,3,4-thia diazoles were synthesized.The preliminary bio-active test shows that these compounds exhibit high antifungal activity.
NaIO4-Catalyzed Bromination of the Aromatic Ring of Lappaconitine
Qiao Hong CHEN , Feng Peng WANG
2001, 12(5): 421-424
[Abstract](474) [FullText HTML] [PDF 38KB](5)
Abstract:
Treatment of lappaconitine 1 with NaIO4 and Br2-HOAc at room temperature for 7 h afforded smoothly the bromine-containing derivative 4 in 71% yield.
Synthesis of Glucoside Bonded Metal Porphyrins
Zao Ying LI , Xun Jin ZHU , Li LI , Yue Ning ZHANG
2001, 12(5): 425-428
[Abstract](442) [FullText HTML] [PDF 35KB](0)
Abstract:
The reactions of 5,10,15,20-tetrakis (p-hydroxyphenyl) porphyrin 1 and 5-(p-hydroxy-phenyl)-10,15,20-tris (p-methoxyphenyl) porphyrin 2 with 1-bromo-2,3,4,6-O-acetyl-α-D-glu-coside 3 respectively afforded 5,10,15,20-tetrakis [p-(2,3,4,6-O-acetyl-glucoside)-1-O-phenyl] porphyrin 4 and 5,10,15-tris (p-methoxyphenyl)-20-[p-(2,3,4,6-O-acetyl-glucoside)-1-O-phenyl] porphyrin 5.Their metal complexes Co (4),Mn (4) and Co (5),Mn (5) also have been prepared.These new compounds have been identified by IR,UV-visible,1H NMR spectra and elemental analysis.
A New Abietane Diterpenoid from the Barks of Taxus yunnanensis
Sheng Hong LI , Hong Jie ZHANG , Ping YAO , Han Dong SUN
2001, 12(5): 429-430
[Abstract](434) [FullText HTML] [PDF 21KB](0)
Abstract:
The structure of a new abietane diterpenoid,taxayunnin (1),from the barks of Taxus yunnanensis,was determined by spectroscopic analysis.A known abietane diterpenoid,taxamairin C (2),was also isolated.
A New Perylenequinone from Hypomyces sp.
Wei Zhong LIU , Yun Xiu SHEN , Xiang Feng LIU , Yuan Teng CHEN , Jin Lun XIE
2001, 12(5): 431-432
[Abstract](461) [FullText HTML] [PDF 26KB](4)
Abstract:
A new perylenequinone,named hypomycin A,was isolated from the mycelia of Hypomyces sp..Its structure was elucidated on the basis of spectroscopic methods.
Two New Xanthone Glycosides from Swertia Tetraptera
Zhi Xin LIAO , Yu Lin LI , Ming Kui WANG , Li Sheng DING , Yao Zu CHEN
2001, 12(5): 433-434
[Abstract](462) [FullText HTML] [PDF 26KB](0)
Abstract:
Two new xanthone glycosides,tetraswerosides A and B,were isolated from the whole plant of Swertia tetraptera.Their structures were determined as 3-O-b-D-glucopyranosyl-1-hydroxy-4,7-dimethoxyxanthone and 3-O-[b-D-xylopyranosyl-(1→6)-b-D-glucopyranosyl]-1-hydroxy-4,7-dimethoxyxanthone by spectroscopic methods.
Four Novel Hydropyranoindeno-Derivatives from Marine Fungus Aspergillus versicolor
Wen Han LIN , Jun LI , Hong Zheng FU , Peter PROKSCH
2001, 12(5): 435-438
[Abstract](476) [FullText HTML] [PDF 33KB](8)
Abstract:
From the cultured filtrates of fungus Aspergillus versicolor,isolated from marine sponge Xestospongia exigua,four novel secondary metabolites,namely aspergillone 1,aspergillodiol 2, aspergillol 3 and 12-acetyl-aspergillol 4,have been isolated by column chromatographic separation.The structures of all the new compounds are established on the basis of extensive 2D NMR spectroscopy in conjugation with MS,UV spectral analysis.The basic structure pattern of those compounds possessed an hydroindenoisopyran nucleus.
Preparation of Zirconia Based Packing Material and Its Evaluation
Xiang Na JIA , Jun Jiao YANG , Yu Min ZUO
2001, 12(5): 439-442
[Abstract](458) [FullText HTML] [PDF 43KB](0)
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A new reversed-phase packing (C18-PBD-ZrO2) was prepared by depositing and cross-linking 1-octadecene (ODE or C18) and polybutadiene (PBD) onto the surface of porous zirconia microspheres (5~10 mm in diameter) which were synthesized by a sol-gel process. These novel column packings possess high mechanical and chemical stability,wider usable pH range and can be used to separate basic compounds with no observable peak tailing.
High Performance Affinity Chromatography of Antithrombin Ⅲ Based on Monodisperse Poly (glycidyl methacrylate) Beads
Ying Xin ZHAO , Di Hua SHANGGUAN , Rui ZHAO , Tian Sheng SHU , Guo Quan LIU
2001, 12(5): 443-446
[Abstract](456) [FullText HTML] [PDF 33KB](0)
Abstract:
A new approach for the separation of antithrombin Ⅲ with high performance affinity chromatography (HPAC) was described. A novel monodisperse,non-porous,cross-linked poly (glycidyl methacrylate) beads (PGMA) were used as the affinity support. With the water-soluble carbodiimide,heparin was linked covalently to amino-PGMA-beads,which was prepared by amination of PGMA. The adsorbent obtained exhibits high binding activity to antithrombin Ⅲ (ATⅢ),good resolution and excellent mechanical properties and can be used under high flow rate.
Resolution of DL-Pantolactone with Ethyldiamine Bridged Dimer Permethyβ-Cyclodextrin as GC Stationary Phase
Dan Ni TAO , Xue Yan SHI , Jun Ling GU , Ruo Nong FU
2001, 12(5): 447-448
[Abstract](454) [FullText HTML] [PDF 22KB](0)
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Ethyldiamine bridged dimer permethy-β-CD and other cyclodextrins were used as GC stationary phase to resolute DL-pantolactone.It is found that this CD dimer has a good selectivity for DL-pantolactone.
In Vitro Interaction of Nicotine and Hemoglobin under Liver Cell Metabolizing Condition
Yan WANG , Hong Fang SUN , Hai Fang WANG , Yuan Fang LIU
2001, 12(5): 449-452
[Abstract](461) [FullText HTML] [PDF 36KB](0)
Abstract:
he in vitro interaction of nicotine and hemoglobin (Hb) in a metabolizing system was studied by spectroscopy assays. Visible spectra showed two isobestics,and fluorescence spectra showed static quenching with increasing of nicotine dose. Meanwhile,the CD spectra intensity reduced,showing the conformation of Hb varied markedly through the interaction.All these results suggested that the interaction of nicotine or its metabolites and Hb might do harm to physicological function of Hb.
A Novel Method for Fabrication of a Glass-Electrode-Based Lipase Sensor
Xi Rong HUANG , Yue Zhong LI , Guo Liang YANG , Li Li LIU , Yin Bo QU , Wen Juan ZHANG
2001, 12(5): 453-456
[Abstract](447) [FullText HTML] [PDF 24KB](1)
Abstract:
Based on an unusual reversible sol-gel transition phenomenon,a novel method for the fabrication of a lipase electrode was developed.The response characteristics of the biosensor was studied by potentiometric technique using olive oil as substrate.After optimization,the lipase electrode demonstrated high activity and good stability.
Langmuir-Blodgett Films and Calcium Ion Coordination of Biliverdin and Its Amphiphilic Derivatives
Jian Ming OUYANG
2001, 12(5): 457-460
[Abstract](434) [FullText HTML] [PDF 36KB](0)
Abstract:
Monolayer formation and LB film fabrication of amphiphilic derivative of biliverdin 1,diododecyl biliverdinamide [B(CONHC12H25)2,2] at an air-water interface on pure water subphase and subphase containing calcium ion were investigated and compared with 1.The coordination in ordered molecular films is much different from that in bulk solution.The formation of ligand-calcium complex was confirmed by X-ray photoelectron spectroscopy.
A Novel Bimetallic Tetrahedron Cobalt Complex Promot-ing the Addition of Diethylzinc to Benzaldehyde
Wei Qiang ZHANG , Zhi CHEN , Yu Hua ZHANG , Xin Yi ZHU , Yu Gang CHEN , Huan Wang JING , Yuan Qi YIN
2001, 12(5): 461-464
[Abstract](451) [FullText HTML] [PDF 32KB](0)
Abstract:
Our recent work found a novel bimetallic tetrahedron cobalt complex which can cataly-ze the addition of diethylzinc to benzaldehyde effectively.
The Magnetic Field Effect on the Polymerization of Styrene in Supercritical Carbon Dioxide
Jun LIU , Hong Ping LI , Zhi Min LIU , Bu Xing HAN , Hai Ke YAN
2001, 12(5): 465-466
[Abstract](452) [FullText HTML] [PDF 17KB](0)
Abstract:
Styrene was polymerized in supercritical (sc) CO2 with benzoyl peroxide (BPO) as initiator.It was found that the polymerization was accelerated by the external magnetic field.
An Observation on the Microphase Separation of Poly (methyl methacrylate)-block-Polystyrene Copolymer
Jie DENG , Xin Song LI , Zheng Mei WANG , Gang SHAO , Ju Zheng LIU
2001, 12(5): 467-470
[Abstract](458) [FullText HTML] [PDF 43KB](0)
Abstract:
The phase behavior of a well-defined poly (methyl methacrylate)-b-polystyrene block copolymer was studied by transmission electron microscope.The results show that a microphase transition may have occurred in the copolymer film.A kind of lamellae and an ordered bicontinuous double-diamond morphology are observed clearly.The lamellar morphology reveals a larger period of about 400 nm.
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