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1993 Volume 4 Issue 2
1993, 4(2): 95-96
Abstract:
Twenty-seven oxadiazolino[5,4-d][1,5]benzodiheteropine derivatives have been synthesized bythe 1,3-dipolar cycloaddition of benzodiheteropines with nitrile oxide 1,3-dipoles,their conformations andthe characteristics of the newly formed oxadiazoline fused on them have been studied.It has also beenfound that the mass spectra show characteristic fragmentation patterns.
Twenty-seven oxadiazolino[5,4-d][1,5]benzodiheteropine derivatives have been synthesized bythe 1,3-dipolar cycloaddition of benzodiheteropines with nitrile oxide 1,3-dipoles,their conformations andthe characteristics of the newly formed oxadiazoline fused on them have been studied.It has also beenfound that the mass spectra show characteristic fragmentation patterns.
1993, 4(2): 97-98
Abstract:
A dodecapeptide extracted from rape pollen was synthesized using solid-phase method,its conformations in different states were studied by FT-IR,CD,and its physiological activities were determined.Sevensegments and five analogs were also synthesized to elucidate the structure-function relation.
A dodecapeptide extracted from rape pollen was synthesized using solid-phase method,its conformations in different states were studied by FT-IR,CD,and its physiological activities were determined.Sevensegments and five analogs were also synthesized to elucidate the structure-function relation.
1993, 4(2): 99-100
Abstract:
11α-Hydroxy-and 11β-chloro-artemisinin have been prepared from artemisinin
11α-Hydroxy-and 11β-chloro-artemisinin have been prepared from artemisinin
1993, 4(2): 101-104
Abstract:
Diadenylyl sulfites were obtained by the condensation of protected adenosines using O,O-bis (1-ben-zotriazolyl) sulfite as a coupling reagent.
Diadenylyl sulfites were obtained by the condensation of protected adenosines using O,O-bis (1-ben-zotriazolyl) sulfite as a coupling reagent.
1993, 4(2): 105-106
Abstract:
The first total synthesis of(-)-3-oxoeudesma-1,4,11(13)-trien-7αH-12-oic acid 1 has been described.The key step is one-pot reaction involving dehydrogenation and allylic oxidationwith selenium dioxide.
The first total synthesis of(-)-3-oxoeudesma-1,4,11(13)-trien-7αH-12-oic acid 1 has been described.The key step is one-pot reaction involving dehydrogenation and allylic oxidationwith selenium dioxide.
1993, 4(2): 107-108
Abstract:
A new method for aromatization of 5(10)-steroidal C3-dimethyl ketalswith pyridinium hydrobromide perbromide （PHP.Py·HBr·Br2） to aromatic A ring steroids in high yield （90-95%） is described.
A new method for aromatization of 5(10)-steroidal C3-dimethyl ketalswith pyridinium hydrobromide perbromide （PHP.Py·HBr·Br2） to aromatic A ring steroids in high yield （90-95%） is described.
1993, 4(2): 109-110
Abstract:
Promoted by various reductants,the addition of 1-iodo-4-chloro-perfluorobutane to 1-hexene giving 1:1 adduct is reported.Based on these facts,several new redox systems are proposed.
Promoted by various reductants,the addition of 1-iodo-4-chloro-perfluorobutane to 1-hexene giving 1:1 adduct is reported.Based on these facts,several new redox systems are proposed.
1993, 4(2): 111-114
Abstract:
Solid state photochemical reactions of antipyrine with 5-formyl-1,3-dimethyluracil,p-nitrobenzaldehyde and p-hydroxybenzaldehyde have been described.The structuresof 4 hey compounds obtained were determined by IR,UV,1HNHR,ns and elemental analysis.
Solid state photochemical reactions of antipyrine with 5-formyl-1,3-dimethyluracil,p-nitrobenzaldehyde and p-hydroxybenzaldehyde have been described.The structuresof 4 hey compounds obtained were determined by IR,UV,1HNHR,ns and elemental analysis.
1993, 4(2): 115-118
Abstract:
Photochemical reactions of 3-methylindole,carbazole,benzimidazole with fusedpolycyclic aromatic hydrocarbons in solid state were investigated,The structures of 4 newcompounds were confirmed by IR,UV,1HNNR,MS and elemental analysis.The structure of compounds 3.6 was established by X-ray crystallography.
Photochemical reactions of 3-methylindole,carbazole,benzimidazole with fusedpolycyclic aromatic hydrocarbons in solid state were investigated,The structures of 4 newcompounds were confirmed by IR,UV,1HNNR,MS and elemental analysis.The structure of compounds 3.6 was established by X-ray crystallography.
1993, 4(2): 119-120
Abstract:
(TPP)OAc was obtained by refluxing Ga2O3 and the free base TPPH2 in acetic acid containing sodium acetate in a yield of 65%.
(TPP)OAc was obtained by refluxing Ga2O3 and the free base TPPH2 in acetic acid containing sodium acetate in a yield of 65%.
1993, 4(2): 121-122
Abstract:
Metal clusters RCCoa（CO）9（R-H,C1,Br,CHa,Ph） were preparedin 18.8-57.3% yields from the reaction of cobalt(Ⅱ)salt and RCXa under mild PTC conditions(latm CO,25℃).The cobalt salt was reducedto Co（CO）4 in the presence of NaaS2O4.
Metal clusters RCCoa（CO）9（R-H,C1,Br,CHa,Ph） were preparedin 18.8-57.3% yields from the reaction of cobalt(Ⅱ)salt and RCXa under mild PTC conditions(latm CO,25℃).The cobalt salt was reducedto Co（CO）4 in the presence of NaaS2O4.
1993, 4(2): 123-124
Abstract:
Dibenzoyl peroxide undergoes oxidative addition on metallic copper powder with 2,2'-bipyridine(or imidazole)in a mixed solvent（methanol and tetrahydrofuran）,and affords the Cu(Ⅱ) complexes-[Cu(C6H5COO)2（2,2’-bipy）]H2O(1) and [Cu(C6H5COO)2(CaH4N2)2 ](2).The structure was solved by direct methodsand Fourier synthesis.C24H20N2O5Cu (1),Mr=479.78,space group P2(1)/c,a=6.986(7),b=18.833(I),c=17.021(3)Å,α=γ=90°,Z=4,V=2218.Å3,Dc=1.443g/cm3,R=0.055Rw=0.062.Complex(2),C20H18N4O4Cu(2),Mr=441.74,space group P2（1）/n,a=8.699(4),b=9.840(6),c=12.399Å(5),α=γ=90°,β=100.8°,Z=4,V=1010.9Å3,Dc=1.654g/cma,R=0.055,Rw=0.062.
Dibenzoyl peroxide undergoes oxidative addition on metallic copper powder with 2,2'-bipyridine(or imidazole)in a mixed solvent（methanol and tetrahydrofuran）,and affords the Cu(Ⅱ) complexes-[Cu(C6H5COO)2（2,2’-bipy）]H2O(1) and [Cu(C6H5COO)2(CaH4N2)2 ](2).The structure was solved by direct methodsand Fourier synthesis.C24H20N2O5Cu (1),Mr=479.78,space group P2(1)/c,a=6.986(7),b=18.833(I),c=17.021(3)Å,α=γ=90°,Z=4,V=2218.Å3,Dc=1.443g/cm3,R=0.055Rw=0.062.Complex(2),C20H18N4O4Cu(2),Mr=441.74,space group P2（1）/n,a=8.699(4),b=9.840(6),c=12.399Å(5),α=γ=90°,β=100.8°,Z=4,V=1010.9Å3,Dc=1.654g/cma,R=0.055,Rw=0.062.
1993, 4(2): 125-128
Abstract:
A new aromatic thermotropic liquid crystalline polyester-ether sulfone(PEES) was prepared from 4,4-bis(4-hydroxyphenoxy)diphenyl sulfone(BHPDS),terephthalic acid(TPA)and p-hydroxybenzoic acid(P-HBA).Some factors that affected melting viscosity of polymer such as prepolymerization reaction medium and post-polymerization etc,were discussed.The liquid crystalline properties were characterized by DSC,polarizing microscope with a hot stage and WAXD measurements.
A new aromatic thermotropic liquid crystalline polyester-ether sulfone(PEES) was prepared from 4,4-bis(4-hydroxyphenoxy)diphenyl sulfone(BHPDS),terephthalic acid(TPA)and p-hydroxybenzoic acid(P-HBA).Some factors that affected melting viscosity of polymer such as prepolymerization reaction medium and post-polymerization etc,were discussed.The liquid crystalline properties were characterized by DSC,polarizing microscope with a hot stage and WAXD measurements.
1993, 4(2): 129-132
Abstract:
A new series of thermotropic liquid crystalline poly(ester-imide)s were synthesized via a solution polycondensation process.The polymers were also characterized by IR,DSC,polarizing microscopy and WAXD measurements.
A new series of thermotropic liquid crystalline poly(ester-imide)s were synthesized via a solution polycondensation process.The polymers were also characterized by IR,DSC,polarizing microscopy and WAXD measurements.
1993, 4(2): 133-136
Abstract:
Two new oleanane type saponins wereisolated from the alcoholic extract of the bark of Nothopanax davidii(Franch) Harms(Araliaceae).Their structures have been determined on th e basis of spectral and chemical data as 3-O-β-(2',4'-O-diacetyl)-D-xylopyranosyl-3β-hydroxyolean-12-ene-28,29-dioicacid-28-O-[α-L-rhamnopyranosyl(1-4)-β-D-glucopyranosyl(1-6)-β-D-glucopyranosyl] ester(1),named yiyeliangwanoside VII;3-O-β-(3'-O-acetyl)-D-xylopyranosyl-3β-hydroxyolean-12-ene-28,29-dioic acid-28-O-[α-L-rhamnopyranosyl(1-4)-β-D-glucopyranosyl(1-6)-β-D-glucopyranosyl] ester(Ⅱ),named yiyeliangwanoside Ⅷ.
Two new oleanane type saponins wereisolated from the alcoholic extract of the bark of Nothopanax davidii(Franch) Harms(Araliaceae).Their structures have been determined on th e basis of spectral and chemical data as 3-O-β-(2',4'-O-diacetyl)-D-xylopyranosyl-3β-hydroxyolean-12-ene-28,29-dioicacid-28-O-[α-L-rhamnopyranosyl(1-4)-β-D-glucopyranosyl(1-6)-β-D-glucopyranosyl] ester(1),named yiyeliangwanoside VII;3-O-β-(3'-O-acetyl)-D-xylopyranosyl-3β-hydroxyolean-12-ene-28,29-dioic acid-28-O-[α-L-rhamnopyranosyl(1-4)-β-D-glucopyranosyl(1-6)-β-D-glucopyranosyl] ester(Ⅱ),named yiyeliangwanoside Ⅷ.
1993, 4(2): 137-138
Abstract:
Two minor steroidal saponins were isolated from the roots of Smilax menispermoidea.One of them is new and its structure was established as(25S) spirost-5-en-3β,17α,27-triol-3-O-[α-L-rhamnopyranosyl(1-4)]-β-D-gluco-pyranoside using spectroscopic and chemical methods.
Two minor steroidal saponins were isolated from the roots of Smilax menispermoidea.One of them is new and its structure was established as(25S) spirost-5-en-3β,17α,27-triol-3-O-[α-L-rhamnopyranosyl(1-4)]-β-D-gluco-pyranoside using spectroscopic and chemical methods.
1993, 4(2): 139-140
Abstract:
Three novel interesting polychlorinated cyclodipeptides,designated dyssmide A(1),B(2),C(3)and a known compound,2,3-dihydrodyeamide C(4) were isolated from the sponge Dysidea sp.Their structures were elucidated by spectroscopic methods.
Three novel interesting polychlorinated cyclodipeptides,designated dyssmide A(1),B(2),C(3)and a known compound,2,3-dihydrodyeamide C(4) were isolated from the sponge Dysidea sp.Their structures were elucidated by spectroscopic methods.
1993, 4(2): 141-144
Abstract:
Two new furostanol saponins,named macrostemonoside E(1) and F(2), were isolated from the bulbs of Allium macrostemon Bunge (Liliaceae),their structures were established oy spectroscopic analysis and chemical evidences.Both possessed strong inhibitory activity on human platelet aggregation.
Two new furostanol saponins,named macrostemonoside E(1) and F(2), were isolated from the bulbs of Allium macrostemon Bunge (Liliaceae),their structures were established oy spectroscopic analysis and chemical evidences.Both possessed strong inhibitory activity on human platelet aggregation.
1993, 4(2): 145-148
Abstract:
A novel hasubanan alkaloid has been isolated along with the known aknadinine from the fresh roots of Stephania sutchenensis.Its structure has been established as 1-nitroaknadinine from detailed spectral studies and confirmed by chemical correlation with aknadinine.The novel alkaloid is the first nitro-hasubanan and also the first example of naturally occurring nitro-alkaloids.
A novel hasubanan alkaloid has been isolated along with the known aknadinine from the fresh roots of Stephania sutchenensis.Its structure has been established as 1-nitroaknadinine from detailed spectral studies and confirmed by chemical correlation with aknadinine.The novel alkaloid is the first nitro-hasubanan and also the first example of naturally occurring nitro-alkaloids.
1993, 4(2): 149-152
Abstract:
A serial of fullerenes had been built and the optimized geometries had been obtained with the energy minimization of molecular mechanics calculations according to the fact that the pentagonal number is exactly 12 in the fullerenes which consist of pentagons and hexagons.The fullerene geometry prediction could facilitate further theoretical and synthetical studies in the near future.
A serial of fullerenes had been built and the optimized geometries had been obtained with the energy minimization of molecular mechanics calculations according to the fact that the pentagonal number is exactly 12 in the fullerenes which consist of pentagons and hexagons.The fullerene geometry prediction could facilitate further theoretical and synthetical studies in the near future.
1993, 4(2): 153-156
Abstract:
The inclusion crystal formed by the hexamethylenamine with p-nitrophenol has a layer type structure,and is divided organic layer and inorganic layer,the latter has a width of 1.0136nm.Metal ions can enter hydrated layer of the crystal,the contents of the cations and water in the crystal are determined.The XRD analysis of the layer type structure of the crystal is also given.
The inclusion crystal formed by the hexamethylenamine with p-nitrophenol has a layer type structure,and is divided organic layer and inorganic layer,the latter has a width of 1.0136nm.Metal ions can enter hydrated layer of the crystal,the contents of the cations and water in the crystal are determined.The XRD analysis of the layer type structure of the crystal is also given.
SPECTROPHOTOMETRIC ANALYSIS OF MIXTURES OF TRACE METAL BY DOUBLE-SYSTEM AND MULTIVARIATE CALIRRATION
1993, 4(2): 157-158
Abstract:
In this paper,a new method for simultaneous spectrophotometric analysis of multicomponent with double-system was developed.The multivariate calibration method,principal component analysis-partial least squares(PCA-PLS),was described and applied to the processing of measurement data.A demonstration,simultaneous determination of cobalt,nickel,copper,zinc and iron with double-system(5-Br-PADAP and PAR as chromogenic chelate reagents,respectively) was given.The results showed that the method with douhle-system gave better precision than those with single system and MLR(in this paper,AKC method was selected)did not give satisfied precision in any situation.
In this paper,a new method for simultaneous spectrophotometric analysis of multicomponent with double-system was developed.The multivariate calibration method,principal component analysis-partial least squares(PCA-PLS),was described and applied to the processing of measurement data.A demonstration,simultaneous determination of cobalt,nickel,copper,zinc and iron with double-system(5-Br-PADAP and PAR as chromogenic chelate reagents,respectively) was given.The results showed that the method with douhle-system gave better precision than those with single system and MLR(in this paper,AKC method was selected)did not give satisfied precision in any situation.
1993, 4(2): 159-162
Abstract:
For the superconductors(RbxK1-x)3C60（x=0.1）,according to BCS theory and assuming that the virtual phonon acting on electron-pair is corresponding to the intrasolecular vibration in the bnckminnterfullerene C60,a linear relationship of the superconducting transition temperature Tc with x has been derived,which is in agreement with the experimentals,
For the superconductors(RbxK1-x)3C60（x=0.1）,according to BCS theory and assuming that the virtual phonon acting on electron-pair is corresponding to the intrasolecular vibration in the bnckminnterfullerene C60,a linear relationship of the superconducting transition temperature Tc with x has been derived,which is in agreement with the experimentals,
1993, 4(2): 163-166
Abstract:
Sulfonated polyphenylene-sulfide（SPPS）was used as ligands in place of phosphine in Rh-complexes to yield a water-soluble catalyst for hydroformylation of higher olefins in two phasic system.The decreasing catalytic activities and increasing n/b ratios（normal to branch aldehyde ratios）have been found respectively with increasing molar ratios of SPPS to rhodium,and with lowering of reaction temperature,indicating more or less coordinations between thioether sulfides and Rh species in SPPS-Rh compounds,The coordinations were also evidenced by a weak Reman hand observation of the SPPS-Rh compounds at 264 cm-1.
Sulfonated polyphenylene-sulfide（SPPS）was used as ligands in place of phosphine in Rh-complexes to yield a water-soluble catalyst for hydroformylation of higher olefins in two phasic system.The decreasing catalytic activities and increasing n/b ratios（normal to branch aldehyde ratios）have been found respectively with increasing molar ratios of SPPS to rhodium,and with lowering of reaction temperature,indicating more or less coordinations between thioether sulfides and Rh species in SPPS-Rh compounds,The coordinations were also evidenced by a weak Reman hand observation of the SPPS-Rh compounds at 264 cm-1.
1993, 4(2): 167-170
Abstract:
The adsorption of CO on Fe(110)with different coverages of titania has been studied by AES,XPS,UPS.It is proposed that the adsorption sites of CO in this system are not only blocked by the deposited TiOX,but also by the products of the dissociation of CO which is promoted by the deposited TiOX.
The adsorption of CO on Fe(110)with different coverages of titania has been studied by AES,XPS,UPS.It is proposed that the adsorption sites of CO in this system are not only blocked by the deposited TiOX,but also by the products of the dissociation of CO which is promoted by the deposited TiOX.
1993, 4(2): 171-174
Abstract:
The calculations on the ground state x~ 1∑+g and two excited states Ã3B2, B~ 1B2 of MgH2 system are carried out by using SOCI (Second Order Configuration Interaction)method[1]. For each state,the electronic structure and related properties are investigated,The vibration and localization analyses are also performed.The reasonable explanations of bending geometries for the excited states are given.
The calculations on the ground state x~ 1∑+g and two excited states Ã3B2, B~ 1B2 of MgH2 system are carried out by using SOCI (Second Order Configuration Interaction)method[1]. For each state,the electronic structure and related properties are investigated,The vibration and localization analyses are also performed.The reasonable explanations of bending geometries for the excited states are given.
1993, 4(2): 175-178
Abstract:
A self-consistent-field-configuration interaction（SCF-CI）procedure of studying highly excited vibrational states of bent triatomic molecules is suggested and its application to O3 is investigated.
A self-consistent-field-configuration interaction（SCF-CI）procedure of studying highly excited vibrational states of bent triatomic molecules is suggested and its application to O3 is investigated.
1993, 4(2): 179-180
Abstract:
A calcium ion-setective eletrode based on a new neutral carrier was studied.The electrode gives a Nernstian response in the rang 5.9-1 Pa and the response is stable in a wide pH range.Logarithms of setectivity coefficents are -2.3 Li(+),-3.5 Na(+),-4.0 K(+),-3.7NH4(+),-4.5 Mg(2+) and-4.4 Zn(2+).
A calcium ion-setective eletrode based on a new neutral carrier was studied.The electrode gives a Nernstian response in the rang 5.9-1 Pa and the response is stable in a wide pH range.Logarithms of setectivity coefficents are -2.3 Li(+),-3.5 Na(+),-4.0 K(+),-3.7NH4(+),-4.5 Mg(2+) and-4.4 Zn(2+).
1993, 4(2): 181-182
Abstract:
Complex of meso-tetra-(1-naphthyl) tetrabenzo-porphyrin with holmium acetylacetonate,Ho(TNTBP)acac(TNTBP:meso-tetra-(1-naphthyl) tetrabenzoporphyrin.Hacac:acetylacetone) have been prepared and characterized by elemental analyses,ultra-violet visible spectra and infrared spectra.
Complex of meso-tetra-(1-naphthyl) tetrabenzo-porphyrin with holmium acetylacetonate,Ho(TNTBP)acac(TNTBP:meso-tetra-(1-naphthyl) tetrabenzoporphyrin.Hacac:acetylacetone) have been prepared and characterized by elemental analyses,ultra-violet visible spectra and infrared spectra.
1993, 4(2): 183-186
Abstract:
Time-resolved fluorescence spectra of europium methylbenzoates（MBA）with 1,10-phenanthroline（phen）have been measured at room temperature.For each of the europium chelates,where the ligand triple states lie above the 5D1 level of Eu3-,the spectra providc evidence that the Eu3- 5D0 state is populated by nonradiative energy transfer from the higher-lying 5D1state.The relaxation time for energy decay from 5D1 state is measured in the microcrystals to bc of the order of a few microseconds.It is suggested that the ligand C=0 and C=C stretching vibrations and Eu-O vibrations,chclate ring and benzene ring vibrations make important contributions to the relaxation process.The 5D1-5D0 relaxation time of Eu(p-MBA)3phen is shorter than those of Eu(m-MBA)3phen and Eu(o-MBA)3phen since nonradiative degradation to 5D0 from 5D1 appears to be more strongly influenced by the Eu3+ sites in the former.
Time-resolved fluorescence spectra of europium methylbenzoates（MBA）with 1,10-phenanthroline（phen）have been measured at room temperature.For each of the europium chelates,where the ligand triple states lie above the 5D1 level of Eu3-,the spectra providc evidence that the Eu3- 5D0 state is populated by nonradiative energy transfer from the higher-lying 5D1state.The relaxation time for energy decay from 5D1 state is measured in the microcrystals to bc of the order of a few microseconds.It is suggested that the ligand C=0 and C=C stretching vibrations and Eu-O vibrations,chclate ring and benzene ring vibrations make important contributions to the relaxation process.The 5D1-5D0 relaxation time of Eu(p-MBA)3phen is shorter than those of Eu(m-MBA)3phen and Eu(o-MBA)3phen since nonradiative degradation to 5D0 from 5D1 appears to be more strongly influenced by the Eu3+ sites in the former.
1993, 4(2): 187-188
Abstract:
The dynamic 1H and 1aC-NMR studies on [Li（2D）][Nd(ηa-C3H5)4]（D=dioxane）were reported The four allyls coordinated to Hd8+ ion are equivalent and hydrogens appear as three groups in 1H-NMR spectra with their chemical shifts changing with temperature.C1 and Ca are equivalent showing the characteristic of η2-allyl.The paramagnetic shifts of carbons in allyls induced by Nd2+ ere separated sucessfully.C1 and C3 located on the zero-dipolar cone.The content of contact shift is greater than that of dipolar slift to Co.
The dynamic 1H and 1aC-NMR studies on [Li（2D）][Nd(ηa-C3H5)4]（D=dioxane）were reported The four allyls coordinated to Hd8+ ion are equivalent and hydrogens appear as three groups in 1H-NMR spectra with their chemical shifts changing with temperature.C1 and Ca are equivalent showing the characteristic of η2-allyl.The paramagnetic shifts of carbons in allyls induced by Nd2+ ere separated sucessfully.C1 and C3 located on the zero-dipolar cone.The content of contact shift is greater than that of dipolar slift to Co.
