Login In
1994 Volume 5 Issue 8
1994, 5(8): 643-644
Abstract:
Two new 19-and 20-member macrocycles containing nitrogen,oxygen and sulfur heteroatoms were synthesized by the nontemplate method starting from thiophene and α, ω-dialkylamine under high-dilution conditions.Hg(Ⅱ), Pb(Ⅱ) and Cd(Ⅱ) complexes of L1 were also prepared.
Two new 19-and 20-member macrocycles containing nitrogen,oxygen and sulfur heteroatoms were synthesized by the nontemplate method starting from thiophene and α, ω-dialkylamine under high-dilution conditions.Hg(Ⅱ), Pb(Ⅱ) and Cd(Ⅱ) complexes of L1 were also prepared.
1994, 5(8): 645-646
Abstract:
β-CD 2-O-and 3-O-monobenzoate were synthesised by direct benzoylation of β-CD with benzoyl chloride in alkaline aqueous solution.
β-CD 2-O-and 3-O-monobenzoate were synthesised by direct benzoylation of β-CD with benzoyl chloride in alkaline aqueous solution.
1994, 5(8): 647-650
Abstract:
A new series of amphiphiles of monoalkyl azotic crown ethers has been synthesized.TEM,DSC and UV-Vis spectroscopy of aqueous dispersions of these amphiphiles indicate that they can form self-assembly of bilayer membranes when dispersed in water.
A new series of amphiphiles of monoalkyl azotic crown ethers has been synthesized.TEM,DSC and UV-Vis spectroscopy of aqueous dispersions of these amphiphiles indicate that they can form self-assembly of bilayer membranes when dispersed in water.
1994, 5(8): 651-654
Abstract:
Three Ebselen derivatives (Ⅲ1-3) were designed and synthesized with amino acid attached to the p-position of 2-phonyl moiety.Effect of compound Ⅱ,Ⅲ1,Ⅲ2,Ⅲ2,as well as Ebselen on the Fe3+/cysteine-induced rat microsomal lipid peroxidation were investigated.And their IC50 were 30,17.7,22.7,22.2 and 24 μmol/L respectively.
Three Ebselen derivatives (Ⅲ1-3) were designed and synthesized with amino acid attached to the p-position of 2-phonyl moiety.Effect of compound Ⅱ,Ⅲ1,Ⅲ2,Ⅲ2,as well as Ebselen on the Fe3+/cysteine-induced rat microsomal lipid peroxidation were investigated.And their IC50 were 30,17.7,22.7,22.2 and 24 μmol/L respectively.
1994, 5(8): 655-658
Abstract:
A series of compounds had been synthesised from 1.6-anhydro-2,4-di-O-benzyl-β-D-glucopyranose with good yields.The effects of C-3 protecting groups on ring-opening reaction and the glycosidation of α-D-glucopyranosyl bromides were studied.
A series of compounds had been synthesised from 1.6-anhydro-2,4-di-O-benzyl-β-D-glucopyranose with good yields.The effects of C-3 protecting groups on ring-opening reaction and the glycosidation of α-D-glucopyranosyl bromides were studied.
1994, 5(8): 659-662
Abstract:
The rearrangement of 3-butylphthalide and its two homologues to 5-carboxyl-1-alkyltetrahydronaphthalene by 1,4-hydride transfer and 3-propylphthalide to 4-carboxyl-1-alkylindane by 1,3-hydride transfer in the presence of AlCl3 were observed and the possible mechanism was discussed.
The rearrangement of 3-butylphthalide and its two homologues to 5-carboxyl-1-alkyltetrahydronaphthalene by 1,4-hydride transfer and 3-propylphthalide to 4-carboxyl-1-alkylindane by 1,3-hydride transfer in the presence of AlCl3 were observed and the possible mechanism was discussed.
1994, 5(8): 663-666
Abstract:
N-Bromomethyl-N-methyl-1,2,3,4-tetrahydro-iso-quinolinium bromide(1) reacted with sodium 2,6-di-tert-butylphenoxide to afford compound 2a,3a,4 and 5 via the benzylic N-ylide intermediate.Meanwhile,when compound 1 reacted with tri-n-butylphosphine,the coupling compound 7 was obtained via demethylation reaction.The reaction mechanisms were discussed.
N-Bromomethyl-N-methyl-1,2,3,4-tetrahydro-iso-quinolinium bromide(1) reacted with sodium 2,6-di-tert-butylphenoxide to afford compound 2a,3a,4 and 5 via the benzylic N-ylide intermediate.Meanwhile,when compound 1 reacted with tri-n-butylphosphine,the coupling compound 7 was obtained via demethylation reaction.The reaction mechanisms were discussed.
1994, 5(8): 667-670
Abstract:
Eight of three different kinds of long absorption wavelength dyes with typical structures have been chosen for studying the relation between structure and stability.The three kinds of dyes are quinocyanine.naphthothiacarbocyanine and carbocyanines.The environmental effect,such as light,oxygen and water,has been investigated.Results show that quinocyanine dyes prefer to hydrolytic reaction,while naphthothiacarbocyanine dyes tend to oxidizing reaction and photo-oxidation reaction process in singlet oxygen mechanism.
Eight of three different kinds of long absorption wavelength dyes with typical structures have been chosen for studying the relation between structure and stability.The three kinds of dyes are quinocyanine.naphthothiacarbocyanine and carbocyanines.The environmental effect,such as light,oxygen and water,has been investigated.Results show that quinocyanine dyes prefer to hydrolytic reaction,while naphthothiacarbocyanine dyes tend to oxidizing reaction and photo-oxidation reaction process in singlet oxygen mechanism.
1994, 5(8): 671-672
Abstract:
Chemical investigation of O-Zhang-Ye fuzi,cultivated Aconitum carmichaeli Debx.,from Zhong-Ba,Sichuan,resulted in the isolation of a new alkaloid,aldohypaconitine (1),along with the known alkaloids:hypaconitine (2),mesaconitine,aconitine,neoline,fuziline,songorine,and songoramine.Songoramine has not been reported previously in this plant.The structure of 1 has been established on the basis of spectral methods,and confirmed by chemical correlation with hypaconitine (2).
Chemical investigation of O-Zhang-Ye fuzi,cultivated Aconitum carmichaeli Debx.,from Zhong-Ba,Sichuan,resulted in the isolation of a new alkaloid,aldohypaconitine (1),along with the known alkaloids:hypaconitine (2),mesaconitine,aconitine,neoline,fuziline,songorine,and songoramine.Songoramine has not been reported previously in this plant.The structure of 1 has been established on the basis of spectral methods,and confirmed by chemical correlation with hypaconitine (2).
1994, 5(8): 673-674
Abstract:
A new flavonol glycoside,caohuoside 5 was isolated from the aerial parts of Epimedium koreanum.Its structure was determined by spectroscopic methods(FAEMS,EIMS,1E NMR,1E-1H COSY,1H-1H TCCSY,13C NMR,APT,1H-13C CCSY and 1H-13C long range COSY) and chemical evidences.
A new flavonol glycoside,caohuoside 5 was isolated from the aerial parts of Epimedium koreanum.Its structure was determined by spectroscopic methods(FAEMS,EIMS,1E NMR,1E-1H COSY,1H-1H TCCSY,13C NMR,APT,1H-13C CCSY and 1H-13C long range COSY) and chemical evidences.
1994, 5(8): 675-678
Abstract:
A new p-acetytphenyl glycoside,asterbatanoside A has been isolated from the roots of Aster batangensis,and its structure has been elucidated as p-hydroxyacetophenone-O-β-D-xylopyranosyl-(1-6)-β-D-glucopyranoside by chemical and spectral means.For the confirmation of this structure,the synthesis of this compound was also reported in this paper.
A new p-acetytphenyl glycoside,asterbatanoside A has been isolated from the roots of Aster batangensis,and its structure has been elucidated as p-hydroxyacetophenone-O-β-D-xylopyranosyl-(1-6)-β-D-glucopyranoside by chemical and spectral means.For the confirmation of this structure,the synthesis of this compound was also reported in this paper.
1994, 5(8): 679-680
Abstract:
Aluminium has been determined by β-correction spectrophotometry with phenylfluorone (PF)and a non-ionic surfactant,emulsifying OP in pH 8 ammoniacal buffer solution.β-correction spectrophotometric method can eliminate completely the effect of excess PF to increase the analytical sensitivity and decrease error.The results have shown that Beer's law was obeyed over the concentration range 0-15 μg Al(Ⅲ)/25 ml and the relative standard deviation was less than 3.3%.
Aluminium has been determined by β-correction spectrophotometry with phenylfluorone (PF)and a non-ionic surfactant,emulsifying OP in pH 8 ammoniacal buffer solution.β-correction spectrophotometric method can eliminate completely the effect of excess PF to increase the analytical sensitivity and decrease error.The results have shown that Beer's law was obeyed over the concentration range 0-15 μg Al(Ⅲ)/25 ml and the relative standard deviation was less than 3.3%.
1994, 5(8): 681-684
Abstract:
Electrostatic Pseudo Liquid Membrane (ESPLIM),developed in this laboratory,is a novel chemical separation technique.In this paper,a study has been conducted on extraction and preconcentration of scandium from dilute aqueous solution by ESPLIM.The effects were studied on the scandium extraction of the extractant,applied field,the pH value of feed and scandium concentration in the feed.The extraction efficiency of scandium from feed containing 25-100 mg/L of scandium was more than 99%.and scandium was concentrated from 21.64 mg/L in the feed to 2474 mg/L in the concentrate,giving a concentration factor of 114.The experimental results demonstrated that the concentration of scandium in the organic phase was much lower than its equilibrium concentration in the solvent extraction,which confirms the nonequilibrium feature of the ESPLIM process.ESPLIM seems to be a very convenient,effective and economic method for extracting and preconcentrating scandium.
Electrostatic Pseudo Liquid Membrane (ESPLIM),developed in this laboratory,is a novel chemical separation technique.In this paper,a study has been conducted on extraction and preconcentration of scandium from dilute aqueous solution by ESPLIM.The effects were studied on the scandium extraction of the extractant,applied field,the pH value of feed and scandium concentration in the feed.The extraction efficiency of scandium from feed containing 25-100 mg/L of scandium was more than 99%.and scandium was concentrated from 21.64 mg/L in the feed to 2474 mg/L in the concentrate,giving a concentration factor of 114.The experimental results demonstrated that the concentration of scandium in the organic phase was much lower than its equilibrium concentration in the solvent extraction,which confirms the nonequilibrium feature of the ESPLIM process.ESPLIM seems to be a very convenient,effective and economic method for extracting and preconcentrating scandium.
1994, 5(8): 685-686
Abstract:
A number of researcher have found that the catalytic properties of metal oxides can be promoted by adding of halides, especially metal chlorides and bromides[1-3]. But the utilizing of fluorides, which should be more stable than the corresponding chlorides and bromides under the conditions of OCM reaction, has not been reported. In this paper the promoting effect of fluoride on OCM reaction was studied.
A number of researcher have found that the catalytic properties of metal oxides can be promoted by adding of halides, especially metal chlorides and bromides[1-3]. But the utilizing of fluorides, which should be more stable than the corresponding chlorides and bromides under the conditions of OCM reaction, has not been reported. In this paper the promoting effect of fluoride on OCM reaction was studied.
1994, 5(8): 687-688
Abstract:
In situ FT-IR of SiO2-supported(PPh3)HPt(μ-PPh2)(μ-CO)Mo(CO)4heterobiuclear hydrido carbonyl catalyst in tbe CO hydrogenation condition has been investigated.
In situ FT-IR of SiO2-supported(PPh3)HPt(μ-PPh2)(μ-CO)Mo(CO)4heterobiuclear hydrido carbonyl catalyst in tbe CO hydrogenation condition has been investigated.
1994, 5(8): 689-692
Abstract:
The catalyst system,CP2TiCl2/n-BuLi,exhibits very high activity for the hydrogenation of 1-octene with a maximum turnover frequency of 71 sec-1.Factors which strongly affect the activities of this catalyst system have been discussed.
The catalyst system,CP2TiCl2/n-BuLi,exhibits very high activity for the hydrogenation of 1-octene with a maximum turnover frequency of 71 sec-1.Factors which strongly affect the activities of this catalyst system have been discussed.
1994, 5(8): 693-694
Abstract:
Studies of the photopolymerization of mesogenic monomer[4-(2-methylpropenoyloxy)-4'-cyanobiphenyl](CBK-M) under the action of a DC electric field have been performed.The influence of the applied voltage on the srereostructure of the polymers obtained was observed.It is explained to be due to the interaction of cyanobiphenyl mesogenic groups with the electric field.
Studies of the photopolymerization of mesogenic monomer[4-(2-methylpropenoyloxy)-4'-cyanobiphenyl](CBK-M) under the action of a DC electric field have been performed.The influence of the applied voltage on the srereostructure of the polymers obtained was observed.It is explained to be due to the interaction of cyanobiphenyl mesogenic groups with the electric field.
1994, 5(8): 695-696
Abstract:
In this paper,The 3-line in solid and 12-line high-viscosity solution ESR spectra of the propagating radical of Polystyrene were studied.The 3-line spectrum comes from the conformation of the radical R1 which usually corresponds to a 6-line typical spectrum but appear as an apparent 3-line spectrum in solid state.The 12-line spectrum comes from two species of radicals with the same confomation R2 but different G factor.R2 corresponds to a 8-line typical spectrum which appear as an apparent 6-line spectrum in the high-viscosity solution.Therefore,two apparent 6-line spectra of R2 with different g values form the 12-line spectrum.
In this paper,The 3-line in solid and 12-line high-viscosity solution ESR spectra of the propagating radical of Polystyrene were studied.The 3-line spectrum comes from the conformation of the radical R1 which usually corresponds to a 6-line typical spectrum but appear as an apparent 3-line spectrum in solid state.The 12-line spectrum comes from two species of radicals with the same confomation R2 but different G factor.R2 corresponds to a 8-line typical spectrum which appear as an apparent 6-line spectrum in the high-viscosity solution.Therefore,two apparent 6-line spectra of R2 with different g values form the 12-line spectrum.
1994, 5(8): 697-700
Abstract:
The heterobinuclear complex of formula Cu(oxap)Gd(phen)2(ClO4)3 has been synthesized,where oxap denotes the N,N'-bis (2-aminopropyl) oxamido dianion and phen represents 1,10-phenanthroline.The complex was characterized with ESR and variable temperature magnetic susceptibility (4-300K).The least-squares fit of the experimental susceptibilities yielded J=2.25cm-1.The observed Gd(Ⅲ)-Cu(Ⅱ) coupling is ferromagnetic.One plausible mechanism that can cause a ferromagnetic coupling between Gd(Ⅲ) and Cu (Ⅱ) is discussed in terms of spin-polarization.
The heterobinuclear complex of formula Cu(oxap)Gd(phen)2(ClO4)3 has been synthesized,where oxap denotes the N,N'-bis (2-aminopropyl) oxamido dianion and phen represents 1,10-phenanthroline.The complex was characterized with ESR and variable temperature magnetic susceptibility (4-300K).The least-squares fit of the experimental susceptibilities yielded J=2.25cm-1.The observed Gd(Ⅲ)-Cu(Ⅱ) coupling is ferromagnetic.One plausible mechanism that can cause a ferromagnetic coupling between Gd(Ⅲ) and Cu (Ⅱ) is discussed in terms of spin-polarization.
1994, 5(8): 701-702
Abstract:
The results of the photoelectron spectra for the oxysulfide glasses in the Li2S-B2O3(-LiBr) systems are discussed.The peak resolved S2p spectra show the existences of bridging and non-bridging S.The values of the binding energy of Lils indicate the chemical environmemts of Li+ ions.
The results of the photoelectron spectra for the oxysulfide glasses in the Li2S-B2O3(-LiBr) systems are discussed.The peak resolved S2p spectra show the existences of bridging and non-bridging S.The values of the binding energy of Lils indicate the chemical environmemts of Li+ ions.
1994, 5(8): 703-706
Abstract:
In the previous paper,the geometry of the triatomic clusters for Cu,Ag,and Au was obtained using the DV-Xα method.In this investigation the atomic orbital interactions of atom Cu,Ag,Au in the triatomic clusters are analyzed.The magnitudes of the atomic orbital interactions of the atoms in the clusters are measured by the splitting of corresponding atomic orbital.The calculation results show the atomic orbital interactions of Cu triatomic cluster differ greatly from those of Ag and Au triatomic cluster because of the mixture radio of 4s-orbital with 3d-orbital in the Cu cluster more than those in the Ag and Au cluster.The values of atomic orbital interactions of Au in the cluster are larger than corresponding atomic orbital interactions of Ag in the cluster.
In the previous paper,the geometry of the triatomic clusters for Cu,Ag,and Au was obtained using the DV-Xα method.In this investigation the atomic orbital interactions of atom Cu,Ag,Au in the triatomic clusters are analyzed.The magnitudes of the atomic orbital interactions of the atoms in the clusters are measured by the splitting of corresponding atomic orbital.The calculation results show the atomic orbital interactions of Cu triatomic cluster differ greatly from those of Ag and Au triatomic cluster because of the mixture radio of 4s-orbital with 3d-orbital in the Cu cluster more than those in the Ag and Au cluster.The values of atomic orbital interactions of Au in the cluster are larger than corresponding atomic orbital interactions of Ag in the cluster.
1994, 5(8): 707-710
Abstract:
The lattice damage produced in GaAs and Al0.3Ga0.7As/GaAs superlattices by 1 MeV Si+ irradiation at room temperature and elevated temperature was investigated by using Rutherford backscattering/channeling (RBS/C) technique and the results of the damage accumulation observed in the experiment are explained by the relative bond strength obtained from molecular-orbital calculation of a group of atomic cluster simulated GaAs and AlxGa1-xAs/GaAs.
The lattice damage produced in GaAs and Al0.3Ga0.7As/GaAs superlattices by 1 MeV Si+ irradiation at room temperature and elevated temperature was investigated by using Rutherford backscattering/channeling (RBS/C) technique and the results of the damage accumulation observed in the experiment are explained by the relative bond strength obtained from molecular-orbital calculation of a group of atomic cluster simulated GaAs and AlxGa1-xAs/GaAs.
1994, 5(8): 711-712
Abstract:
A complex polymer[Cu2(oxen)(pic)(H2O)]N(ClO4)·ZnH2O,where oxen and pic are N,N'-bis(2-aminoethyl)oxamide and pyridine-4-carboxylate,respectively,was synthesized.It crystallizes in the monoclinic space group P21/c,with a=10.420(2) Å,b=13.118(2) Å,c=14.863(5) Å,β=93.05(2)°,and z=4.The structure of this complex consists of 2D network of copper(Ⅱ) ions bridged by bis-tridentate oxen in trans-conformation,and by pyridine-4-carboxylate in which the pyridine ring acts as a monodentate group whereas the carboxylate as a tridentate group and bonds to three different copper centres in a novel fashion.The repeating asymmetric unit is a binuclear copper(Ⅱ) fragment with one of the copper centre locating in a lengthening octahedral environment,whereas the other in a distorted tetragonal pyramid geometry.
A complex polymer[Cu2(oxen)(pic)(H2O)]N(ClO4)·ZnH2O,where oxen and pic are N,N'-bis(2-aminoethyl)oxamide and pyridine-4-carboxylate,respectively,was synthesized.It crystallizes in the monoclinic space group P21/c,with a=10.420(2) Å,b=13.118(2) Å,c=14.863(5) Å,β=93.05(2)°,and z=4.The structure of this complex consists of 2D network of copper(Ⅱ) ions bridged by bis-tridentate oxen in trans-conformation,and by pyridine-4-carboxylate in which the pyridine ring acts as a monodentate group whereas the carboxylate as a tridentate group and bonds to three different copper centres in a novel fashion.The repeating asymmetric unit is a binuclear copper(Ⅱ) fragment with one of the copper centre locating in a lengthening octahedral environment,whereas the other in a distorted tetragonal pyramid geometry.
1994, 5(8): 713-714
Abstract:
The synthesis and crystal structure are reported for the sheet-like compound[CU2(oxpn)Fe(CN)5(NO)]■,where oxpn is the dianion of N,N'-bis(3-aminopropyl)oxamide.This compound crystallizes in the orthogonal space group Pnma,with a=11.413(4),b=22.242(5),c=7.736(2) Å,and Z=4.The structure was refined to conventional discrepancy factors R=0.047 and Rw=0.054.The Cu(Ⅱ) and Fe(Ⅲ)centors are bridged by oxpn and cyanide,the former behaves as a bis-terdentate ligand bound to copper(Ⅱ) ion to form copper(Ⅱ) dimers,whereas the latter bridges Cu(Ⅱ) and Fe(Ⅲ) centers in both symmetric and asymetric end-to-end bis-monodentate fashions,spreading out along be plane to form a 2D network.The structure is made up of CuFe unit with Cu(Ⅱ) and Fe(Ⅲ) ions locating in a distorted square-based pynamic and a compressed octahedron,respectively.
The synthesis and crystal structure are reported for the sheet-like compound[CU2(oxpn)Fe(CN)5(NO)]■,where oxpn is the dianion of N,N'-bis(3-aminopropyl)oxamide.This compound crystallizes in the orthogonal space group Pnma,with a=11.413(4),b=22.242(5),c=7.736(2) Å,and Z=4.The structure was refined to conventional discrepancy factors R=0.047 and Rw=0.054.The Cu(Ⅱ) and Fe(Ⅲ)centors are bridged by oxpn and cyanide,the former behaves as a bis-terdentate ligand bound to copper(Ⅱ) ion to form copper(Ⅱ) dimers,whereas the latter bridges Cu(Ⅱ) and Fe(Ⅲ) centers in both symmetric and asymetric end-to-end bis-monodentate fashions,spreading out along be plane to form a 2D network.The structure is made up of CuFe unit with Cu(Ⅱ) and Fe(Ⅲ) ions locating in a distorted square-based pynamic and a compressed octahedron,respectively.
1994, 5(8): 715-716
Abstract:
Ru3(CO)12 entrapped within NaY zeolite cages was prepared by monolayer dispersion technique,which can be reversibiy decarbonylated and recarbonyiated.
Ru3(CO)12 entrapped within NaY zeolite cages was prepared by monolayer dispersion technique,which can be reversibiy decarbonylated and recarbonyiated.
1994, 5(8): 717-718
Abstract:
The early-late transition metal heterobinuclear Pt-M(M=Cr,Mo,W)hydrido carbonyl compounds were synthesized and characterized by IR and NMR spectroscopic means.
The early-late transition metal heterobinuclear Pt-M(M=Cr,Mo,W)hydrido carbonyl compounds were synthesized and characterized by IR and NMR spectroscopic means.
1994, 5(8): 719-720
Abstract:
The synthesis and characterization of the previously unknown P2W17(NbO2)O617-,a new composition containing one NbvO2 peroxide group,was described,O22- of the molecule was detected by I-/S2O32- titration.the structure of the anion prepared was characterized by elementel analysis,IR,UV and 31P-NMR spectra.
The synthesis and characterization of the previously unknown P2W17(NbO2)O617-,a new composition containing one NbvO2 peroxide group,was described,O22- of the molecule was detected by I-/S2O32- titration.the structure of the anion prepared was characterized by elementel analysis,IR,UV and 31P-NMR spectra.
