1995 Volume 6 Issue 3

A NOVEL CYCLODIMERIZATION OF α,β- UNSATURATED KETONES PROMOTED BY LOW-VALENT TITANIUM
Long Hu ZHOU , Gui Yuan DAI , Da Qing SHI , Wen Bin SHEN
1995, 6(3): 173-176
[Abstract](159) [FullText HTML] [PDF 108KB](0)
Abstract:
Low-valent titanium reagent prepared from titanium tetrachloride and zinc in tetrahydrofuran has been used to promote a novel cyclodimerization of α,β-unsaturated ketones,leading to cyclopentanol derivatives(2 and3).A possible reaction mechanism was proposed.
ACID CATALYZED REARRANGEMENTS OF TRIQUINANES
Cong ZHANG , Xiao Chuan GUO , Xiu Min SHEN , Yong Fen XU
1995, 6(3): 177-180
[Abstract](170) [FullText HTML] [PDF 115KB](0)
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Acid catalyzed rearrangements of 1 and 3 were examined.The olefinic double bond was the most reactive group in protonation reaction.In the absence of olefinic double bond,tert-hydroxy group reacted faster than cyclopropane ring.
STUDY ON THE MANNICH-TYPE REACTION OF P-TOLUENESULFONAMIDE
Ru Yu CHEN , Qing DAI
1995, 6(3): 181-184
[Abstract](166) [FullText HTML] [PDF 115KB](1)
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The Mannich-type reactions of p-toluenesulfonamide with trichlorophosphine,dichlorophenylphosphine,diethyl phosphite,or triphenylphosphite were studied.The structures of new products were confirmed by 1HNMR,31PNMR,MS,elemental analysis and x-ray diffraction.
A FACILE METHOD FOR THE O-GLYCOSIDATION OF BENZOYL SUBSTITUTED HETEROCYCLIC KETENE AMINALS
Zhan Jiang LI , Li Ben WANG , Zhi Tang HUANG
1995, 6(3): 185-188
[Abstract](157) [FullText HTML] [PDF 107KB](0)
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Heterocyclic ketene aminals 1 or 2 reacted with 2,3,4,6-tetra-O-acetyl-a-D-glucopyranosyl bromide using mercuric cyanide-calcium hydride or mercuric cyanide-molecular sieve 4A as catalyst to give the O-glycosidated heterocyclic ketene aminals 3 or 4 in moderate yields.
STUDIES ON THE STEREO-AND ENANTIOSELECTIVE SYNTHESIS OF 11.12-EPOXYSARCOPHYTOL-A, 11, 12-EPOXYSARCOPHYTOL-A ACETATE AND 11, 12-EPOXYCEMBRENE-C.-SYNTHESIS OF 5,9,13-TRIMETHYL-2-ISOPROPYL-12(S), 12(S)-EPOXY-141-BROMO-2(Z) ,4(E)- 8(E)-TETRADECATRIENENITRILE
Xiang Jun YUE , Ting Hao LI , Yu Lin LI
1995, 6(3): 189-192
[Abstract](181) [FullText HTML] [PDF 103KB](1)
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An efficient synthesis of 5,9,13-trimethyl-2-isopropyl-12(S),13(S)-epoxy-14-bromo-2(Z),4(E),8(E)-tetradecatrienenitrile,a key intermediate in the synthesis of antitumor cembranoids including 11,12-epoxy-sarcophytol-A,11,12-epoxysarcophytol-A acetate and 11,12-epoxycembrene-C,was first described through seven step sequence in~32% overall yield from E,E-farnesol.
SYNTHESIS OF ANALOGUES OF HUPERZINE A 3.THE PREPARATION OF SOME SINGLE RING ANALOGUES OF HUPERZINE A
Bao Gen WU , Wei Pin ZHEN , Yun Xin BO , Xu Chang HE , Dong Lu BAI
1995, 6(3): 193-196
[Abstract](162) [FullText HTML] [PDF 142KB](0)
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Huperzine A(1),an inhibitor of acetylcholinesterase isolated from the clubmoss Huperzia serrata,is used for treatment of Alzheimer's disease.The preparation of four analogues of Hup A,compounds 2,3,4 and 5,was described.Their biological activities were also tested.
SYNTHESIS OF 4-S-(1“-ARYL-TETRAZOLE-5”-YL)-4-DEOXY-4'-DEMETHYL-EPIPODOPHYLLOTOXIN ANALOGUES
Kuan Ke LU , Fang Min LIU , Yao Zu CHEN
1995, 6(3): 197-198
[Abstract](166) [FullText HTML] [PDF 64KB](0)
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As continuation of our study,6 title compouds were synthesized by condensing 1-aryl-5-mercapto-tetrazoles with 4'-demethyl-epipodophyllotoxin in the presence of CF3COOH(TFA).
REACTION OF C60 AND 2-AMINO-ETHYLHYDROGENSULFATE
Liang Bing GAN , De Jian ZHOU , Chu Ping LUO , Chun Hui HUANG , Jin Qi PAN , Mu Jian LÜ , Yi WU
1995, 6(3): 199-200
[Abstract](169) [FullText HTML] [PDF 80KB](0)
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C60 reacts with 2-aminoethylhydrogensulfate to give a mixtore of mono-and bispiperazine fullerene adducts C60(C4H8N2)1-2 and a water-soluble f'ullerene derivative C60Hn(NHCH2CH2OSO3Na)n.
PREPARATION AND CHARACTERIZATION OF A NEW HEXAHYDROPYRROLIZINE DERIVATIVE OF FULLERENE
Hone Xian HAN , Yu Liang LI , Yong Fang LI , Ming Yong HAN , Zi WU , Yi Ming MO , Fend Lian BAI , Dao Ben ZHU
1995, 6(3): 201-204
[Abstract](163) [FullText HTML] [PDF 96KB](0)
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C60 undergoes 1,3-dipolar cycloaddition reaction with the 1,3-dipole derived from heating 4-hydroxy-L-proline and paraformaldehyde to form a monoadduct in yield of 29.3%.
SYNTHESIS OF N-ARYL-4-METHYLPHENOXYACETAMIDES BY MEANS OF LIQUID-LIQUID PHASE TRANSFER CATALYSIS
Tai Bao WEI , Ji Chou CHEN , You Ming ZHANG , Lai Lai WANG
1995, 6(3): 205-208
[Abstract](165) [FullText HTML] [PDF 100KB](0)
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The title compounds 3a-3n were prepared with high yields via the reaction of 4-methylphenoxyacetyl chloride with various substituted aromatic amines under the condition of liquid-liquid phase transfer catalysis using polyethylene glycol-400 as catalyst.
PHOSPHORYL PROMOTION EFFECT AND FORMATION OF BOTH PEPTIDES AND NUCLEOTIDES
yong JU , Wei Hua ZHOU , Yu Fen ZHAO
1995, 6(3): 209-210
[Abstract](163) [FullText HTML] [PDF 96KB](0)
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In the presence of phosphoryl group,N-(O,O-diisopropyl)phosphoryl threonine reacted with nucleosides to give both nucleotides and peptides.The result might give some clue to the prebiotic formation of nucleic acids and proteins.
PEPTIDES FORMATION FROM DIPP-HIS
Yao Wu SHAO , Yu Fen ZHAO
1995, 6(3): 211-214
[Abstract](178) [FullText HTML] [PDF 142KB](0)
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When DIPP-HIS was incubated in water,citrate buffer,DMF and other mixed solvents,phosphoryl dipeptide,tripeptide even tetrapeptide were found.When DIPP-HIS was incubated with aspartic acid under the same condition.cross dipeptide were found.
PHOTOOXIDATION OF SOME ORGANIC COMPOUNDS CATALYZED BY DECATUNGSTATES
Bin YUE , Si San ZHU , Gao Yang XIE , Yi Dong GU
1995, 6(3): 215-216
[Abstract](168) [FullText HTML] [PDF 72KB](0)
Abstract:
Under the action of near-visible and UV light,[W10O32]4- undergoes one and two electrons photoreduction to oxidize organic compounds.In homogeneous systems and in the presence of excess of oxygen,photooxidation of alcohols,amine,cyclic hydrocarbon and alkyl benzenes catalyzed by decatungstates have been studied.
NEOARCTIN A FROM ARCTIUM LAPPA L.
Hai Yan WANG , Jun Shan YANG
1995, 6(3): 217-220
[Abstract](170) [FullText HTML] [PDF 118KB](0)
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A new lignan,neoarctin A,has been isolated from the seeds of Arctium lappa L.,and the structure elucidated on the basis of spectral analyais.
THE STRUCTURE OF ASTERBATANOSIDE J FROM ASTER BATANGENSIS
YU SHAO , BING NAN ZHOU , LONG ZE LIN , GEOFFREY A CORDELL
1995, 6(3): 221-224
[Abstract](167) [FullText HTML] [PDF 190KB](0)
Abstract:
A new medicagenic acid saponin named asterbatanoside J was isolated from the roots of Aster batangensis.On the basis of chemical and spectral studies especially 2D NMR including COSY,HETCOR,HOHAHA,ROESY and HMBC techniques,its structure has been established as 3-O-β-D-glucopyranosyl-(1,6)-β-D-glucopyranosyl-2β,3β-dihydroxy-olean-12-en-23α.28-dioic acid-28-O-α-L-arabinopyranosyl-(1,3)-α-L-rhamnopyranosyl-(1,2)-β-D-fucopyranoside.
TAXAYUNTIN G:A NEW TAXOID FROM TAXUS YUNNANENSIS
Qin YUE , Qi Cheng FANG , Xiao Tian LIANG
1995, 6(3): 225-228
[Abstract](179) [FullText HTML] [PDF 129KB](0)
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A new taxoid,taxayuntin G,was isolated from the leaves and stems of Taxus yunnanensis.Its structure was elucidated by spectroscopic methods(MS,1H-NMR,13C-NMR,1H-1H COSY,1H-13C COSY,NOE and HMBC).
TWO NEW SESQUITERPENES FROM CELASTRUS ORBICULATUS
Ming An Wang , Fu Heng CHEN
1995, 6(3): 229-230
[Abstract](164) [FullText HTML] [PDF 80KB](1)
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Two new β-dihydroagarofuran sesquiterpenes were isolated from Celastrus orbiculatus,their strutures were elucidated as 1α,2α,8β-triacetoxy-9β-cinnamoyloxy-β-dihydro agarofuran(1)and 1α,2α-diacetoxy-6β-benzoyloxy-9β-cinnamoyloxy-β-dihydroagarofuran(2)mainly by spectroscopic methods.
CHEMILUMINESCENCE DETERMINATION OF OXAL ATE
Zhi Ke HE , Rong Ming MA , Qing Yao LUO , Xi Nao YU , Yun E ZENG
1995, 6(3): 231-234
[Abstract](171) [FullText HTML] [PDF 117KB](0)
Abstract:
The reaction between Ru(phen)32-(phen=phenanthroline)and Ce(Ⅳ) produces luminescence in aqueous solution.The effect of oxalate concentration on the intensity of chemiluminescence(CL)emission was firstly studied.CL intensity was linearly related to concentration of oxalate over the range of 3.0×10-8-2.9×10-6 mol/L.The detection limit was 1.5×10-8mol/L.The present paper reports this novel CL method for determination of oxalate,which is usually determined by electrogenerated chemiluminescence method.The method was evaluated by carrying out interference study with common ions and some co-existing compounds in human urine,by a recovery study and by the analysis of oxalate in human urine.The results obtained compared well with reference values.
LACCASE-BASED MICELLAR ENHANCED SPECTROFLUORIMETRIC DETERMINATION OF L-ASCORBIC ACID
Hou Ping HUANG , Ru Xiu CAI , Yu Min DU , Yun E ZENG
1995, 6(3): 235-238
[Abstract](196) [FullText HTML] [PDF 130KB](0)
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An automated flow-injection-stopped-flow micellar enhanced Spectrofluorimetric method for determination of L-ascorbic acid(AA)is described.The method is based on the interference of laccase by AA.causing a decrease in the rate of the laccase-catalysed fluorescence reaction in the presence of Brij-35.The resulting change of fluorescence intensity at em 530nm(ex 430nm)is proportional to the concentration of AA with the linear range over 0.2 to 2.0μg/ml.The significant interference from ferric and cupric ions can be eliminated by addition of ED-TA.The method has been applied to the determination of AA in pharmaceuticals.the results agree well with the nominal values and those obtained by the reference method.The recovery of AA in pharmaceuticals are between 91.5% and 115.4%.
IN SITU RAMAN STUDY OF OXYGEN SPECIES ON BaF2-LaOF CATALYSTS
Zi Sheng CHAO , Xiao Ping ZHOU , Hui Lin WAN , K. R. TSAT
1995, 6(3): 239-242
[Abstract](183) [FullText HTML] [PDF 153KB](0)
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The dioxygen species was characterized and their thermostability was investigated on BaF2-LaOF catalyst by means of in situ Raman spectroscopy in the temperature range of 298K to 1023K.It is found that there exist mainly the O2 2-ions and a little amount of O22-(1 < n < 1)ions at the temperature for OCM(1023K)on BaF2-LaOF catalyst in O2 stream.These dioxygen species can be expected to be the active sites for OCM.
STUDIES ON HOMOGENEOUS SCAVENG REACTION IN CONFINED ETCHANT LAYER TECHNIQUE FOR NANOLITHOGRAPHY (Ⅰ)──As (Ⅲ) SCAVENGING BROMINE REACTION
Lian Yong SU , Jin LUO , Zhong Hua LIN , Zhao Wu TIAN
1995, 6(3): 243-246
[Abstract](161) [FullText HTML] [PDF 104KB](0)
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It is reported that the As(Ⅲ)scavenging bromine reaction rate constant can be determined by means of measuring the limiting current of a rotating disk electrode(RDE).The As(Ⅲ)scavenging bromine second order reaction rate constants in sulfuric acid are 3.6×105Lmol-1·s-1 at 20℃ and 8.9×105 Lmol-1s-1 at 41℃ respectively.The activation energy is 33 KJ·mol-1.The results shows that.As(Ⅲ)can be used as scavenging etchant of bromine in submicronieter and three-dimension lithography.
SYNTHESIS OF A NEW FAMILY OF CHARGE TRANSFER COMPLEXES AND THEIR LANGMUIR FILMS
Yu Fang XIAO , Zhong Qi YAO
1995, 6(3): 247-250
[Abstract](162) [FullText HTML] [PDF 123KB](0)
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Synthesis of a new family of charge transfer complexes-tetramethylthiotetrathiafulvalene-C60Brn)(TMT-TTF-C60Brn,n=6,24) is described.The charge transfer in complexes was investigated by UV electronic absorption spectra.The pressure-area isotherm showed that TMT-TTF-C60Brn) could form stable monolayers at the air-water interface.
STUDIES OF SURFACE PHOTOVOLTAGE PROPERTIES AND CHARGE TRANSFER ON TRANSITION METAL PORPHYRIN COMPLEX (Ⅰ)
Jie ZHANG , De Jun WANG , Tong Shun SHI , Peng ZHANG , Xi Zhang CAO , Tie Jin LI
1995, 6(3): 251-254
[Abstract](174) [FullText HTML] [PDF 185KB](0)
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Photovoltage properties and charge transfer process of tailed porphyrin Mn(Ⅲ) complex,meso-mono-[o-(4-diethylamino)butyramidophenyl] triphenyl porphyrin Mn(Ⅲ)(MDBPTPPMn(Ⅲ)Cl)were investigated by surface photovoltage spectrum(SPS) and field modulation surface photovoltage spectrum(FMSPS).Furthermore,its absorption spectra in near-ultraviolet and near-infrared that have been disputed are given a new assignment in this paper.
SYNTHESIS OF A SILICA-SUPPORTED CARBOXYMETHYL CELLULOSE PLATINUM COMPLEX AND ITS CATALYTIC BEHAVIORS FOR HYDROGENATION OF ETHYL BENZOATE
Li Ming TANG , Mei Yu HUANG , Ying Yan JIANG
1995, 6(3): 255-258
[Abstract](166) [FullText HTML] [PDF 168KB](0)
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A new natural polymeric catalyst,silica-supported carboxymethyl cellulose platinum complex(abbr.as SiO2-CMC-Pt)has been found to catalyze the hydrogenation of ethyl benzoate to ethyl cyclohexanecarboxylate in about 100% yield at 60-70℃ and 1 atm of hydrogen pressure.The turnover number could amount to 925 when reacted for 42 h without deactivation of the catalyst.
DIRECT ELECTROCHEMICAL SYNTHESIS AND CHARACTERIZATION OF SAMARIUM (Ⅲ) COMPLEX WITH 2-HYDROXY-2, 4, 6-CYCLOHEPTATRIENONE (TROPOLONE)
Jian Sheng GU , Jian Ying TONG , Mei Hua MA , Dennis G. TUCK
1995, 6(3): 259-260
[Abstract](168) [FullText HTML] [PDF 101KB](0)
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Tris(tropolonato)samarium(Ⅲ)has been prepared in high yield,by the electrochemical oxidation of samarium metal anode in acetonitrile solution of 2-hydroxy-2,4,6-cycloheptatrienone(tropolone,HL).The unusual divalent samarium(Ⅱ)complex was formed at the first step of electrosynthesis.The final product,Sm(C7H3O3)3,has been characterized by microanalysis and the studies of IR and 1H,13C NMR spectra.
SYNTHESIS AND CHARACTERIZATION OF HETEROBIMETALLIC COMPLEXES: (Cp2LnOCH2C6H5)Cr(CO)3(Ln=Gd,Dy,Yb,Y)
Chang Tao QiAN , Jian Hua GUO
1995, 6(3): 261-260
[Abstract](164) [FullText HTML] [PDF 73KB](0)
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Heterobimetallic complexes in which chromium and lanthanide metals were bridged with difunctional benzyloxide group:(Cp2LnOCH2C6H5)Cr(CO)3(Ln=Gd,Dy,Yb,Y),were synthesized The complexes were characterized by elemental analysis,IR and 1HNMR spectroscopy.
SYNTHESIS AND CRYSTAL STRUCTURE OF THE CLUSTER COMPOUND MoS4CuS2Ag(PhS3P)3Br·HS2O
De Liang LONG , Xin Quan XIN , Xiao Ying HUANG , Jing Hua CAI , Bei Sheng KANG
1995, 6(3): 263-264
[Abstract](166) [FullText HTML] [PDF 85KB](0)
Abstract:
MoS4Cu2Ag(Ph3P)3Br·H2O,fw=1344,triclinic,space group P1:a=13.246(4),b=20.314(6),c=11.995(4)Å,α=93.25(3)°,β=115.99(2)°,γ=74.44(3)°,V=2788.(2)Å3,Z=2,Dc=1.60g cm-3,F(000)=1340,μc=22.87cm-1,R=0.060,RW=0.067.This is the first example of tetranuclear M-Mo-S cluster containing Cu and Ag together and the structure is a completed cubane that the Br atom bonds to Cu and Ag.
SYNTHESIS AND 183W NMR CHARACTERIZATION OF A-β-GeM2W18Ti6O7714 HETEROPOLYANION
Lu MENG , Jing Fu LIU
1995, 6(3): 265-266
[Abstract](179) [FullText HTML] [PDF 77KB](0)
Abstract:
A dimeric Keggin-type polyoxotungstate β-Ge2W18Ti6O7714 has been synthesized from the lacunary precursor β-GeW6O3410 and characterized by means of elemental anajysis,IR,polarogram,183W NMR and FAB mass spectroscopy.The 183W NMR spectrum consists of two lines with intensity ratio 1:2 as expected for trisubstiluted heteropolyanion.With the help of FAB mass spectrum,we concluded that it is a dimer of two Keggin units with D30 symmetry.
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