1993 Volume 4 Issue 6

INSERTION OF PTC-GENERATED DICHLOROCARBENE INTO C-B BO ND.A FACILE SYNTHESIS OF KETONES FROM ALKENES VIA ORGANOBORATES
De Jie ZHAO , Tian Yi KE , Chang Mei KE , Zi Xing SHAN
1993, 4(6): 471-474
[Abstract](47) [FullText HTML] [PDF 182KB](0)
Abstract:
The insertion of dichlorocarbene generated from chloroform by Phase Transfer Catalysis (PTC) into carbon-boron bond of dialkylborate anions 3,obtained by method A and B,resulted in the formation of the intermediates 5,which were oxidized with alkaline hydrogen peroxide to give the corresponding dialkylketones in 36-77.9% yields.
THE SOLID STATE ALDOL CONDENSATION REACTION OF ACETYLFERROCENE AND AROMATIC ALDEHYDES
Ji Ben MEIG , Hong MA , Yong Mei WANG
1993, 4(6): 475-478
[Abstract](81) [FullText HTML] [PDF 131KB](1)
Abstract:
The aldol condensation reactions of acetylferrocene with several aromatic aldehydes have been studied in the solid state.The results showed that they revealed different reactivities in the solid slate from that in solution and eight compounds have been prepared.Their structures have been characterized by UV,IR,1HNMR,HS and elemental analysis.
SELECTIVE REDUCTION OF 3,17-DIOXO-STEROIDS TO 17β-HYDROXY-3-OXO-STEROIDS
Qin Jian ZHAO , Zhen Su LI
1993, 4(6): 479-482
[Abstract](53) [FullText HTML] [PDF 225KB](0)
Abstract:
11β-Hydroxy-androst-4-en-3,17-dione (1a),androst-4,9 (11)-dien-3,17-dione-(2a),androst-4-en-3,11,17-trione (3a),11α-methoxy-androst-4-en-3,17-dione (4a) and 11β-metboxy-androst-4-en-3,17-dione (5a) were selectively reduced to the corresponding 17β-OH derivatives in one step without the protection of 3-oxo (and 11-oxo,in the case of 3a) group with the yields ranging from 65% to 79%.In these reactions,the ditute NaBH4 (or KBH4) solution in methanol was added dropwise to the 3,17-dioxo-steroids solution in methanol-benzene-pyridine,while the reaction mixtures were well stirred at -5~5℃.Acid (such as gtacial acetic acid) was added to quench the reactions.The resulted testosterone derivatives (1b~5b) were purified by flash chromatography.
TOTAL SYNTHESIS OF (+)-7-EPI-GONIDFUFURONE
Zhao Hui ZHOU
1993, 4(6): 483-484
[Abstract](53) [FullText HTML] [PDF 77KB](0)
Abstract:
First total synthesis of natural styryl-furone,(+)-7-epigoniofufurone 1,from D-glycero-D-gulo-heptono-γ-lactone in eight steps (13% overall) is described.The absolute stereochemistry of 1 is confirmed.
SYNTHESIS OF A NEW TYPE OF SCOPOLAMINE ANALOGUES
Guo Hua CHU , Qi Ting ZHOU , Dong Lu BAI , Ru Yun JI
1993, 4(6): 485-488
[Abstract](52) [FullText HTML] [PDF 144KB](0)
Abstract:
A series of compounds,which are structurally analogous to scopolamine and also in accordance with the general formula of neuroleptic benzamides,were synthesized and tested for their potential antipsychotic activity.
ACYLATIVE CLEAVAGE OF CYCLIC ETHERS CATALYZED BY SAMARIUM TRICHLORIDE
Shi Hui WU , Zong Biao DING , Yuan Mei CHEN
1993, 4(6): 489-492
[Abstract](60) [FullText HTML] [PDF 139KB](0)
Abstract:
Oxiranes as well as four and five membered rings of cyclic ethers were cleaved with acyl chloride in the presence of samarium trichloride or Eu (hfe)3 as Lewis-acid catalyst under mild conditions,the oorresponding chloroesters were obtained readily and smoothly in excellent yields.
A SIMPLE AND CONVENIENT ROUTE FOR PREPARATION OF OPTICALLY ACTIVE BICYCLOLACTONES
Hui Jun WU , Qi WEI , Hai Jian SHI , Liang CHEN , Shou Yuan LIN
1993, 4(6): 493-494
[Abstract](55) [FullText HTML] [PDF 95KB](0)
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Optically active bicyclolactones 4 were prepared via a new simple route.
THE PREPARATION OF 5-HYDROXYMETHYLFURFURALDEHYDE FROM FRUCTOSE OR SUCROSE CATALYZED BY ZrCl4
Biao YU , Chuan LI , Yong Zheng HUI
1993, 4(6): 495-496
[Abstract](51) [FullText HTML] [PDF 89KB](0)
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5-Hydroxymethylfurfuraldehyde (HMF) was prepared from fructose or sucrose in high yield by using ZrCl4 or Cp2ZrCl2 as the catalyst under mild conditions.
STRUCTURAL STUDIES OF AN ARABINOGALACTAN——A WATER SOLUBLE POLYSACCHARIDE FROM THE POLLEN OF PAPAVER SOMNIFERUM
Feng HE , Ping MIAO , Sheng JIN
1993, 4(6): 497-498
[Abstract](56) [FullText HTML] [PDF 71KB](0)
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A polysaccharide,PS(1),has been isolated from the pollen of papaver somniferum.PS(1) is a highly branched arabinogalactan,which,mainly contains α-L-arabinofuranosyl(1→)and(3,6→1)-β-D-galactopyranosyl residues.We also studied the circular dichroism and immunoactivity of PS(1).
NEPHTIXAMIDE A AND B FROM THE SOFT CORAL NEPHTHEA TIXIERAE VERSEVELDT
Gui Yong Sheng WANG , Jing Yu SU , Long Mei ZENG
1993, 4(6): 499-500
[Abstract](53) [FullText HTML] [PDF 77KB](0)
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Two new ceramides,Nephtixamide A and B,were isolated from the soft coral Nephthea tixierae verseveldt.Their structures were established by spectroscopic methods.
SALVIANOLIC ACID H,A NEW DEPSIDE FROM SALVIA CAVALERIEI VAR.SIMPLICIFOLIA
Hai Jun ZHANG , Lian Niang LI
1993, 4(6): 501-504
[Abstract](57) [FullText HTML] [PDF 162KB](0)
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A new depside named salvianolic acid H was isolated from the aqueous extract of Salvia cavaleriei var.simplicifolia,along with salvianolic acid A,B,C,isosalvianolic acid C,lithospermic acid,rosmarinic acid,R-(+)-β-(3,4-dihydroxyphenyl) lacticacid and protocatechualdehyde.Rosmarinic acid was obtained as the major component.
NEW MACROCYCLIC COMPOUND,CLEMOCHINENOSIDE B FROM CLEMATIS CHINENSIS
Chun Qing SONG , Ren Sheng XU
1993, 4(6): 505-506
[Abstract](61) [FullText HTML] [PDF 73KB](2)
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The structure of a new macrocyclic compound,clemochinenoside B,isolated from the root of Clematis chinensis was elucidated by means of NMR,FAB-MS,NOE and chemical hydrolysis.
PHOTOPHYSICAL PROPERTIES OF THE ASYMMETRIC PENTAAZADENTATE PORPHYRIN-LIKE MACROCYCLES
Shi Ming DONG , Duo Yuan WANG
1993, 4(6): 507-510
[Abstract](57) [FullText HTML] [PDF 142KB](0)
Abstract:
The porphyrin-like macrocycles and their metal complexes are a novel family of photoresponsive molecules.The properties of the excited states,both singlet and triplet are investigated by the stationary and transient processes.
THE SYNTHESIS AND DIOXYGEN-AFFINITY OF SOME SCHIFF-BASE COBALT (Ⅱ) CHELATES COORDINATIVELY BOUND ON POLY (4-VINYLPYRIDINE-CO-STYRENE)
Jian Biao MA , Cun Xiang ZHAO , Jian Min LI , LI Zhong XU , Bing Lin HE
1993, 4(6): 511-512
[Abstract](48) [FullText HTML] [PDF 106KB](0)
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Some Schiff-base cobalt(Ⅱ) chelates like ethylenebis [(2-hydroxy-3-methoxy-5-methylphenyl)methylideneiminato]Cobalt(Ⅱ) were coordioatively anchored onto poly (4-vinylpyridine-co-styrene) in diglyme solution and the dioxygen-affinity of the resulting polymeric complexes were measured in situ.
THEORETICAL INVESTIGATION OF COLLISION ENERGY EFFECT ON REACTION O BARIUM WITH METHYL BROMIDE
Xi Guang ZHFNG , Ke Li HAN , Ben Fan SUN , Qin Xing LI , Zhen Xin YU , Guo Zhong HE
1993, 4(6): 513-516
[Abstract](48) [FullText HTML] [PDF 145KB](0)
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The reacdynamics on Ba+BrCH3→BaBr+CH3 has been investigated in the first proposed potential energy surface of the generalized LEPS type,using the quasiclassical trajectory method.In simulation of the conditions in molecular beam experiments,the results of the present study show significant effect of the reagent collision energy on the dynamics of the reaction,and are in good agreement with the experimental ones.
THE THEORETICAL STUDIES OF PRODUCT ALIGNMENT OF THE REACTIONS OF Na,F WITH CH3I
Ke Li HAN , Guo Zhong HE , Nan Quan LOU
1993, 4(6): 517-520
[Abstract](62) [FullText HTML] [PDF 120KB](0)
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The NaI and IF product rotational alignment of the reactions of Na,F+CH3I has been theoretically studied in a LEPS PES.The product alignment versus the relative translational energy of the reactants has been obtained.
A NEW APPROACH TO ESTIMATE KINETIC DECOMPOSITION FROM TG-DTG OR DSC CURVE
Yu Ting ZHAO , Jian Hua ZHANG , Tong Shan SUN , Zhao He YANG
1993, 4(6): 521-522
[Abstract](59) [FullText HTML] [PDF 68KB](0)
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This paper reports a new approach to estimate kinetic parameters for the thermal decomposition of the solid state from TG-DTG or DSC curve.Reduced equations are derived for the first tlme.The validity of these equations was demonstrated employing data obtained from the dehydration process of calcium oxalate monohydrate.
SEQUENTIAL OSCILLATIONS IN BrO3--GALLIC ACID-SULFURIC ACID-[Ni(TIM)]2+ SYSTEM
Xiang Da ZHAO , Zhi Qiang XU , Shi Sheng NI
1993, 4(6): 523-526
[Abstract](51) [FullText HTML] [PDF 126KB](0)
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[Ni(TIM)]2+ can act as a catalyst in bromate-gallic acid-sulfuric acid system to produce sequential oscillations have been studied.When bromate solution is added to the reaction mixture,two sets of concentration oscillations take place,the first set is the noncatalyzed oscillation and the second is [Ni(TIM)]2+ catalyzed oscillation.
APPLICATION OF FULLERENES TO THE STUDY ON ITIES Ⅰ:INHIBITION TO THE TRANSFER OF TMA+
Er Kang WANG , Guo Yi ZHU , Zhen Shi CAI , Xin Hua GUO , Zi Yang LIU , Shu Yin LIU
1993, 4(6): 527-530
[Abstract](54) [FullText HTML] [PDF 147KB](0)
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For the first time,fullerenes are applied to the study on the interface between two immisible electrolyte solutions.Experiments show they are a new kind of inhibitors.Obvious inhibitive behavior to the TMA+ transfer across the water/nitrobenzene interface is observed.
STUDIES ON THE VOLTAMMETRIC BEHAVIOR OF EU(Ⅲ)-ALDOPENTOSE AND EU(Ⅲ)-D-RIBOSE-L-AMINO ACIDS COMPLEXES
Liang XU , Hong Xiang WANG , Xiao Xia GAO
1993, 4(6): 531-534
[Abstract](52) [FullText HTML] [PDF 135KB](0)
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The rate of voltammetric reduction of Eu(Ⅲ) in acetate solution was increased by the formation of a complex with ribose,lyxose or arabinose.If a ternary complex of Eu(Ⅲ)-D-ribose-L-phenylanaline formed on the surface of mercury electrode,the redox process of Eu(Ⅲ) became more reversible than that of Eu(Ⅲ)-D-ribose in solution phase.
MODIFIED ELECTRODE WITH SiW12O404- INCORPORATED INTO POLY (4-AMINOAZOBENZEN) FILM
Jun Wei ZHENG , Heng Bin ZHANG
1993, 4(6): 535-536
[Abstract](58) [FullText HTML] [PDF 103KB](0)
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The immobilization of SiW12O404--in poly (4-aminoazobenzene) film was done by electrochemical method.According to the continuous cyclic voltammograms of the modified electrode,it can be determined that SiW12O404--in the polymer is very stable.The paper reports the elecctrochemical properties of the modified electrode,Moreover,it was found that the modified electrode exhibits electrocatalysis for the reaction of oxygen.
ELECTRONIC STRUCTURE OF (C5H5)aCe(OCMea)
Qing Bo MENG , Guan Yang LIN , Chun Ji NIU , Jia Zuan NI
1993, 4(6): 537-540
[Abstract](63) [FullText HTML] [PDF 121KB](0)
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The electronic structure of (C5H5)aCe(OCMea) have been studied by INDO method.Some interesting results hays been obtained.
STRUCTURAL STUDIES ON CRYSTALLINE 3,4-POLYISOPRENE
Hong Fang ZHANG , Zhi GONG , Fo Song WANG
1993, 4(6): 541-542
[Abstract](55) [FullText HTML] [PDF 102KB](0)
Abstract:
In the paper,the structures of the crystalline 3,4-polyisoprene (3,4-PI) which was first synthesized in our institute,were investigated by using Wide Angle X-ray Diffraction (WAXD);Small Angle X-ray Scattering (SAXS) and Laue photography in various polymerization conditions and elongate ratios.It was found that reducing reaction velocity was favourable for crystalline capacity.The polymeric structures were dependent mainly on nitrogen electron donor.The degree of crystallinity and long period were increased with elongate ratio,but crystalline size was decreased.The polymers used in the work belong to inhomogeneous particulate system.The particulate radii were between 35-164A.
CATALYTIC SYNTHESIS OF MAGNESIUM HYDRIDE UNDER ATMOSPHERIC PRESSURE AND ITS DEHYDROGENATION/HYDRGENATION PROPERTIES
Gen Wen LIN , Shi Jian LIAO , Yun XU , Yi Ping ZHANG
1993, 4(6): 543-546
[Abstract](52) [FullText HTML] [PDF 125KB](0)
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The catalytic hydrogenation of magnesium under atmospheric pressure has been optimized so that the reaction can be completed within seven hours. The resulted magnesium hydride is in the form of superfine powder with an average primary particle size of 15 nm. This magnesium hydride exhibits higher dehydrogenation/hydrogenation rates than that obtained under pressure with the same catalyst system.
PREPARATION AND CHARACTERIZATION OF α-H5[GeW9Mo2VO40]·22H2O
Sheng Xian XU , Qing Yin WU , Yu Lin SONG , Shu Kun WANG
1993, 4(6): 547-550
[Abstract](52) [FullText HTML] [PDF 125KB](0)
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A new mixed heteropoly acid,α-H5[GeW9Mo2VO40]·22H2O,bas been prepared and characterized by means of ICP,potentiometric titration,IR and UV spectra,X-ray powder diffraction and thermal analysis.
A NEW RARE-EARTH VANADATE LaBa2V3O11
X.L. WANG , S.X. SHANG , Z.P. AI , H. WANG , H.C. CHEN , M.H. JIANG
1993, 4(6): 551-554
[Abstract](65) [FullText HTML] [PDF 169KB](1)
Abstract:
A new rare-earth vanadate LaBa2V3O11 is synthesized by the conventional solid state reaction.The single phase can be obtained at sintering temperature of 1010℃. The X-ray powder diffraction shows that the new compound has tetragonal structure with cell parameters a of 7.94 and c of 24.27 Å The LaBa2V3O11 can be decomposed to LaVO4.Ba3(VO2)2 and V2O5 by higher sitering temperature than 1010℃.The as-sintered sample is insulator with resistivity of 1012 ohm cm.Furthermore,if the as-sintered sample was annealed under H2 atmosphere,the LaBa2V3O11 decomposed to LaVO3 and BaYO4 despite ofthe lower annealing temperature of 950℃.
DETERMINATION OF DEGREE OF CHARGE TRANSFER IN CONDUCTING LANGMUIR-BLODGETT FILM OF BEDT-TTF-TCNQ
Yu Fang XIAO , Zhong Qi YAO , Dao Sen JIN
1993, 4(6): 555-558
[Abstract](59) [FullText HTML] [PDF 121KB](0)
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A mixed Langmuir-Blodgett film was built up by mixture 1:1 of bis (ethyldithio) tetrathiafulvalene-tetracyanoquinodimethane/stearie acid(BEDT-TTF-TCNQ/SA).A degree of charge transfer(CT)in complex of BEDT-TTF with TCNQ was estimated at 0.477~0,486 by Raman frequencies of central Vc=c and Vc-s,The existence of charge transfer in BEDT-TTF-TCNQ has been confirmed by FTIR and XPS spectroscopy.
EPITAXIAL CRYSTALLIZATION OF LDPE ON IPP
Shong Ke YAN , Jian LIN , De Cai YANG
1993, 4(6): 559-560
[Abstract](35) [FullText HTML] [PDF 259KB](0)
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Epitaxial crystallization of low-density polyethylene (LDPE) on highly oriented isotactic polypropylene (iPP) has been studied by electron microscopy.The results obtained by bright field (BF) electron microscopy and electron diffraction indicate that the LDPE can epitaxially grow on iPP substrate and form cross-hatched lamellae texture.The c axes of LDPE are ±50°apart from the c axes of iPP.The contact plane of two crystals is (010) of iPP and (100) of LDPE.
X-RAY STRUCTURE OF A SEMICONDUCTING ORGANOMETALLIC SALT,[FeCp(Tol)]2[Ni(mnt)2]
Wei Hua ZHOU , Jin Gui QIN , Dao Yu LIU , Ning Hai HU , Zhong Sheng JIN
1993, 4(6): 561-562
[Abstract](53) [FullText HTML] [PDF 82KB](0)
Abstract:
The title compound was prepared and characterized.Its crystal Structurewas determined by X-ray diffraction analysis,and consists of segregated cation and anion stacks in the perpendicular directions.Crystal data:monoclinic, P21/c,Mr=765.21,a=7.882(2)Å,b=15.526(4)Å,c=13.736(2)Å,β=99.87(2)0,V=1656.0(6)Å3,Dc=1.53g/cm3,Z=2,F(000)=780,R=0.040 and Rw=0.056.
Studies on the influence of heat treatment on polyamide-1010 structure
Hong Fang ZHANG , Bao Quan YANG , Li Hua ZHANG , Zhi Shen MO
1993, 4(6): 561-562
[Abstract](47) [FullText HTML] [PDF 96KB](0)
Abstract:
In this work,the influence of heat treatment on Polyamide-1010 structure of aggregation state was studied by using WAXD and SAXS techniques.The results showed that the best crystallinity was obtained nearby T=175℃ for Polyamide-1010 samples with various annealing treatment.Through extrapolating method,the Tg obtained was approximately 58℃.Based on the one-dimensional electron density correlation function of partially crystalline polymers,some structural parameters of Polyamide-1010 were determined by SAXS.
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