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1992 Volume 3 Issue 7
1992, 3(7): 485-488
Abstract:
By optimization of the reaction conditions, the p-acylation of calixarenes by the Friedel-Crafts reaction succeeded in moderate to good yields.
By optimization of the reaction conditions, the p-acylation of calixarenes by the Friedel-Crafts reaction succeeded in moderate to good yields.
1992, 3(7): 489-492
Abstract:
Methyl, ethyl, n-propyl, and benzyl p-hydroxyphenyl ketones and 6-hydroxy-1-tetralone are shown under the condition of ethylene ketal formation to undergo alkyl-carbonyl C-C bondscission, but not with p-hydroxybenzophenone, p-hydroxyisobutyrophenone, and 5-hydroxy-1-indanone. It is suggested that the scissiou is preceded by an aldol condensation.
Methyl, ethyl, n-propyl, and benzyl p-hydroxyphenyl ketones and 6-hydroxy-1-tetralone are shown under the condition of ethylene ketal formation to undergo alkyl-carbonyl C-C bondscission, but not with p-hydroxybenzophenone, p-hydroxyisobutyrophenone, and 5-hydroxy-1-indanone. It is suggested that the scissiou is preceded by an aldol condensation.
1992, 3(7): 493-494
Abstract:
Acyl isocyanate(Ⅰ) was synthesized by the reaction of acyl chloride with lead cyanate in dichloromethane, using pyridine as a catalyst. Then, adding aryl urea(Ⅱ) to acyl isocyanate, 1-acyl-5-aryl-biuret (Ⅲ) can be obtained. 14 compounds have been synthesized by this method.
Acyl isocyanate(Ⅰ) was synthesized by the reaction of acyl chloride with lead cyanate in dichloromethane, using pyridine as a catalyst. Then, adding aryl urea(Ⅱ) to acyl isocyanate, 1-acyl-5-aryl-biuret (Ⅲ) can be obtained. 14 compounds have been synthesized by this method.
1992, 3(7): 495-498
Abstract:
Baimuxinol, a 4-hydroxymethyl agarofuran isolated from Aquilaria Sinensis, was synthsizd. The stereoselectivity of catalytic hydrogenation of dehydrobaimuxino and its derivatives was studied.
Baimuxinol, a 4-hydroxymethyl agarofuran isolated from Aquilaria Sinensis, was synthsizd. The stereoselectivity of catalytic hydrogenation of dehydrobaimuxino and its derivatives was studied.
1992, 3(7): 499-502
Abstract:
The oxidation of pnitrotoluene with electro-generated superoxide ion in the presence or absence of metallo-porphyrins FeTPP, MnTPP and CoTPP in DMF was studied by cyclic voltammetry and controlled potential electrolysis, Metallo-porphyrins as catalysts for electroreduction of O2, they can not only increase yields of p-nitrobensoic acid and selectivities of reaction but also enable the reaction proceed at lower negative potential.
The oxidation of pnitrotoluene with electro-generated superoxide ion in the presence or absence of metallo-porphyrins FeTPP, MnTPP and CoTPP in DMF was studied by cyclic voltammetry and controlled potential electrolysis, Metallo-porphyrins as catalysts for electroreduction of O2, they can not only increase yields of p-nitrobensoic acid and selectivities of reaction but also enable the reaction proceed at lower negative potential.
1992, 3(7): 503-506
Abstract:
Water-soluble Mn (Ⅲ)-porphyrins supported on various carriers as monooxygenase-like catalysts were used for n-Hexane hydroxylation by PhIO. The hydroxylation yields and XPS measurement of the catalysts indicate that the carriers containing-OH groups have favorable steric and electronic effect on Mn-porphyrins. Some influencing factors and the role of carriers are discussed.
Water-soluble Mn (Ⅲ)-porphyrins supported on various carriers as monooxygenase-like catalysts were used for n-Hexane hydroxylation by PhIO. The hydroxylation yields and XPS measurement of the catalysts indicate that the carriers containing-OH groups have favorable steric and electronic effect on Mn-porphyrins. Some influencing factors and the role of carriers are discussed.
1992, 3(7): 507-510
Abstract:
Addition of myrcene and 3-methyl-3-penten-2-one followed by cyclization afforded perfume "Iso-E-Super" with 2-acetyl-2β,3β,8,8-tetramethyl-1,2,3,4,5,6,7,8-octalin as main component on the basis of its spectroscopic data.
Addition of myrcene and 3-methyl-3-penten-2-one followed by cyclization afforded perfume "Iso-E-Super" with 2-acetyl-2β,3β,8,8-tetramethyl-1,2,3,4,5,6,7,8-octalin as main component on the basis of its spectroscopic data.
1992, 3(7): 511-514
Abstract:
Four new alkaloids, didehydroprotostemonine, isoprotostemonine, neostemonine and stemodiol, were isolated from the roots of a Chinese medicinal plant, Stemona japonica, collected form Zhejiang Province, southern China. Their structures were elucidated by extensive spectral analyses.
Four new alkaloids, didehydroprotostemonine, isoprotostemonine, neostemonine and stemodiol, were isolated from the roots of a Chinese medicinal plant, Stemona japonica, collected form Zhejiang Province, southern China. Their structures were elucidated by extensive spectral analyses.
1992, 3(7): 515-516
Abstract:
From the roots of Sanguisorba alpina, a new triterpenoid was isolated and identified as 2-isobutyryloxy-19α, 25-dihydroxyursa-1, 12-dien-28-oic acid by means of spectral methods, named as aipinic acid.
From the roots of Sanguisorba alpina, a new triterpenoid was isolated and identified as 2-isobutyryloxy-19α, 25-dihydroxyursa-1, 12-dien-28-oic acid by means of spectral methods, named as aipinic acid.
1992, 3(7): 517-520
Abstract:
The neuroexcitotoxic nonprotein amino acid β-N-oxalo-L-α, β-diaminopropionic acid (β-N-ODAP) and its isomer α-N-oxalo-L-α, β-diaminopropionic acid (α-N-ODAP) in Panax ginseng C. A. Meyer (cultivated ih Northeastern China), Panax quinquefolius L., Panax notoginseng F.H. Chen (cultivated in Southwestern China), Korean red ginseng and Jilin red ginseng were isolated and identified. Efficient separation and purification methods for β-N-ODAP and α-N-ODAP were developed.
The neuroexcitotoxic nonprotein amino acid β-N-oxalo-L-α, β-diaminopropionic acid (β-N-ODAP) and its isomer α-N-oxalo-L-α, β-diaminopropionic acid (α-N-ODAP) in Panax ginseng C. A. Meyer (cultivated ih Northeastern China), Panax quinquefolius L., Panax notoginseng F.H. Chen (cultivated in Southwestern China), Korean red ginseng and Jilin red ginseng were isolated and identified. Efficient separation and purification methods for β-N-ODAP and α-N-ODAP were developed.
1992, 3(7): 521-524
Abstract:
Three new bicyclooctanoid neolignans, kadsurenin A, kadsurenin B and kadsurenin C were isolated from Piper kadsura (Choisy) Ohwi. Based on the spectroscopic analysis (UV, JR, MS, NMR, and X-ray), their structures were established as 7R, 8R, 3'S, 4'R, 5'R-△s'-3,4-methyienedioxy-5'-methoxy-4'-acetyloxy-2',3',4',5'-tetrahydro-2'-oxo-7.3',8.5'-neolignan; 7R, 8R, 3'S, 4'R, 5'R-△s'-3, 4-methylenedioxy-5'-methoxy-4'-hydroxy-2',3',4',5'-tetrahydro-2'-oxo-7.3', 8.5'-neolignan and 7R, 8R, 3'S, 4'R, 5'R-△s'-3,4,5'-trimethoxy-4'-hydroxy-2',3',4',5',-tetrahydro-2'-oxo-7.3',8.5'-neolignan respectively.
Three new bicyclooctanoid neolignans, kadsurenin A, kadsurenin B and kadsurenin C were isolated from Piper kadsura (Choisy) Ohwi. Based on the spectroscopic analysis (UV, JR, MS, NMR, and X-ray), their structures were established as 7R, 8R, 3'S, 4'R, 5'R-△s'-3,4-methyienedioxy-5'-methoxy-4'-acetyloxy-2',3',4',5'-tetrahydro-2'-oxo-7.3',8.5'-neolignan; 7R, 8R, 3'S, 4'R, 5'R-△s'-3, 4-methylenedioxy-5'-methoxy-4'-hydroxy-2',3',4',5'-tetrahydro-2'-oxo-7.3', 8.5'-neolignan and 7R, 8R, 3'S, 4'R, 5'R-△s'-3,4,5'-trimethoxy-4'-hydroxy-2',3',4',5',-tetrahydro-2'-oxo-7.3',8.5'-neolignan respectively.
IMMOBILIZATION OF AMINOACYLASE FROM ASPERGILLUS ORYZAE ON CHLOROMETHYLATED CROSS-LINKED POLYSTYRENES
1992, 3(7): 525-528
Abstract:
A number of chlorumethylated polystyrenes were synthesized and tried to immobilize aminoacylase from Aspergillus oryzae and many factors which affected immobilized enzyme activity were studied in detail. The results indicated that the immobilized enzyme on support (IAR-1) possessed high enzymatic activity and high stability.
A number of chlorumethylated polystyrenes were synthesized and tried to immobilize aminoacylase from Aspergillus oryzae and many factors which affected immobilized enzyme activity were studied in detail. The results indicated that the immobilized enzyme on support (IAR-1) possessed high enzymatic activity and high stability.
1992, 3(7): 529-530
Abstract:
The thermolysis of (EtO)2P(O)SCF3 was measured by 31P-NMR with external standard method. Kinetic parameters of the reaction, i.e., order, rate constant, pre-exponential, activation energy were obtained. For constant external-standard method, It is better to choose the value of 31P peak area of standard substance slightly greater than the middle value of the area of the measured compounds.
The thermolysis of (EtO)2P(O)SCF3 was measured by 31P-NMR with external standard method. Kinetic parameters of the reaction, i.e., order, rate constant, pre-exponential, activation energy were obtained. For constant external-standard method, It is better to choose the value of 31P peak area of standard substance slightly greater than the middle value of the area of the measured compounds.
1992, 3(7): 531-532
Abstract:
By using the linear combination of the AGP(antisymmetrtzed geminat power) and SPG(sequential product of geminats) functions, an attempt has been made to catcutate the ground state of the LiH molecule. The calculated results show that-the AGP or SPG function gives the same ground state result as their linear combination.
By using the linear combination of the AGP(antisymmetrtzed geminat power) and SPG(sequential product of geminats) functions, an attempt has been made to catcutate the ground state of the LiH molecule. The calculated results show that-the AGP or SPG function gives the same ground state result as their linear combination.
1992, 3(7): 533-534
Abstract:
Reman spectroscopy is used as a tool to monitor the reaction between N,N'-di (pmethyl) monothioxamides and 1,3-diamine trimethylene and to detect the reaction intermediate. By observing changes of 1024 cm-1 C=S band and appearance of a new bend at around 1720 cm-1, the reaction mechanism is discussed.
Reman spectroscopy is used as a tool to monitor the reaction between N,N'-di (pmethyl) monothioxamides and 1,3-diamine trimethylene and to detect the reaction intermediate. By observing changes of 1024 cm-1 C=S band and appearance of a new bend at around 1720 cm-1, the reaction mechanism is discussed.
1992, 3(7): 535-538
Abstract:
A method of synchronous-high-derivative spectfluor for identification of crude oil and fuel oil pollution is studied. The best operation conditions for the 2nd and 4th deriv, are set. To differentiate oil-spill at river and sea, this method is rapid and simple, and the spectra have high resolution power as "fingerprint".
A method of synchronous-high-derivative spectfluor for identification of crude oil and fuel oil pollution is studied. The best operation conditions for the 2nd and 4th deriv, are set. To differentiate oil-spill at river and sea, this method is rapid and simple, and the spectra have high resolution power as "fingerprint".
1992, 3(7): 539-542
Abstract:
Normal Raman Spectra(NRS) of solid PMT (1-phenyl-5-mercaptotetrazole) and MBT (2-mercaptobenzothiazole) and their surface enhanced Raman spectra (SERS) adsorbed on the surface of the silver subcolloidal particles are reported and compared.
It is supposed that PMT adsorbed on silver with both N and S atoms whereas MBT may be adsorbed on silver through S atom.
Normal Raman Spectra(NRS) of solid PMT (1-phenyl-5-mercaptotetrazole) and MBT (2-mercaptobenzothiazole) and their surface enhanced Raman spectra (SERS) adsorbed on the surface of the silver subcolloidal particles are reported and compared.
It is supposed that PMT adsorbed on silver with both N and S atoms whereas MBT may be adsorbed on silver through S atom.
1992, 3(7): 543-546
Abstract:
A clear light-yellow silver sol which has the visible spectral absorption at 390 nm, when adsorbed phenylmercaptotetrazole(PMT) or mercaptobenzothiazole (MBT), has a new absorption at 510-550 nm. It was found that the adsorption of halide ions competes with PMT and MBT. However, halide ions have a completely different influence from PMT and MBT on the spectral absorption of the silver sol. The differences may result from the change of the properties of the surface of the silver subcolloidal particles and from the bond forms combining adsorbates with the substrates.
A clear light-yellow silver sol which has the visible spectral absorption at 390 nm, when adsorbed phenylmercaptotetrazole(PMT) or mercaptobenzothiazole (MBT), has a new absorption at 510-550 nm. It was found that the adsorption of halide ions competes with PMT and MBT. However, halide ions have a completely different influence from PMT and MBT on the spectral absorption of the silver sol. The differences may result from the change of the properties of the surface of the silver subcolloidal particles and from the bond forms combining adsorbates with the substrates.
1992, 3(7): 547-550
Abstract:
A simple model of chromatographic mechanical mechanism is present, and then a scrics of theoretical chromatographic equations and fundamental Formulae are derived. These theoretical equations and formulae not only reserve thermodynamic characteristics in the current fundamental chromatographic formulae, but also introduce one or more kinetic parameter, so it is possible to make the macroscopic-control on the effect of kinetic characteristics on chromatographic system.
A simple model of chromatographic mechanical mechanism is present, and then a scrics of theoretical chromatographic equations and fundamental Formulae are derived. These theoretical equations and formulae not only reserve thermodynamic characteristics in the current fundamental chromatographic formulae, but also introduce one or more kinetic parameter, so it is possible to make the macroscopic-control on the effect of kinetic characteristics on chromatographic system.
1992, 3(7): 551-554
Abstract:
The carbyne compound [Br(CO)2(Py)2Mo(≡CC6H5)] (Py=pyridine) (1a) reacts with Co2(CO)8, Fe2(CO)9 and Mn2(CO)10 to give tetrahedral tri-metal cluster compounds Co2Mo(μ3-CC6H5)Br(CO)8(Py)2 (2), Fe2Mo(μ3-CC6H5)Br(CO)9(Py)2 (3) and Mn2Mo(μ3-CC6H5)Br(CO)10(Py)2 (4)respectively.Tri-metal cluster compound Co2Mo(μ3-CC6H5)Br(CO)8(bipy) (bipy=α,α'dipyridyl) (5) is prepared in a similar reaction sequence from [Br(CO)2(bipy)Mo(≡CC6H5)] (1b) and Co2(CO)8. IR,1H and 13C NMR spectral data of these compounds are reported and discussed.The crystal structure of compound (5) has been determined by X-ray diffraction.
The carbyne compound [Br(CO)2(Py)2Mo(≡CC6H5)] (Py=pyridine) (1a) reacts with Co2(CO)8, Fe2(CO)9 and Mn2(CO)10 to give tetrahedral tri-metal cluster compounds Co2Mo(μ3-CC6H5)Br(CO)8(Py)2 (2), Fe2Mo(μ3-CC6H5)Br(CO)9(Py)2 (3) and Mn2Mo(μ3-CC6H5)Br(CO)10(Py)2 (4)respectively.Tri-metal cluster compound Co2Mo(μ3-CC6H5)Br(CO)8(bipy) (bipy=α,α'dipyridyl) (5) is prepared in a similar reaction sequence from [Br(CO)2(bipy)Mo(≡CC6H5)] (1b) and Co2(CO)8. IR,1H and 13C NMR spectral data of these compounds are reported and discussed.The crystal structure of compound (5) has been determined by X-ray diffraction.
1992, 3(7): 555-558
Abstract:
The complex K3H4GeW9V3O40·8H2O crystallized in a monocliinie system with space group P2, Mr=2784.67, a=11.099(3), b=16.452(4), c=13.534(4), Å,β=108.14°, Z=2,V=2348.49 Å3, F(000)=2456, μ=239.7cm-1, De=3.932 g/cm3. The final R=0.083 for 4528 non-zero reflexions. The structure of anions GeW9V3O409- and GeW9O3410- belongs to A-α-type.
The complex K3H4GeW9V3O40·8H2O crystallized in a monocliinie system with space group P2, Mr=2784.67, a=11.099(3), b=16.452(4), c=13.534(4), Å,β=108.14°, Z=2,V=2348.49 Å3, F(000)=2456, μ=239.7cm-1, De=3.932 g/cm3. The final R=0.083 for 4528 non-zero reflexions. The structure of anions GeW9V3O409- and GeW9O3410- belongs to A-α-type.
1992, 3(7): 559-560
Abstract:
The title complex i-C4H9Co(salen)(Py) (Py=pyridine. salen=dianion of disalicylideneethylenediamine) has been first synthesized. Its crystal structure has been determined by X-ray diffraction method. The crystsis are monoclinic with space group P21/C. The unit cell parametes are presented. The structure has been refined to a final R of 0.038.
The title complex i-C4H9Co(salen)(Py) (Py=pyridine. salen=dianion of disalicylideneethylenediamine) has been first synthesized. Its crystal structure has been determined by X-ray diffraction method. The crystsis are monoclinic with space group P21/C. The unit cell parametes are presented. The structure has been refined to a final R of 0.038.
1992, 3(7): 561-562
Abstract:
The canonical and locatized molecutar orbiters of [NCCuS2NoS2]2- cluster were calculated by means of CNDO quantum chemistry method. Then the energy and properties of corresponding chemicat bonds were discussed, especially, Cu-Sb-No three center conjugated π bonds and No-St-No conjugated π bonds were accounted for.
The canonical and locatized molecutar orbiters of [NCCuS2NoS2]2- cluster were calculated by means of CNDO quantum chemistry method. Then the energy and properties of corresponding chemicat bonds were discussed, especially, Cu-Sb-No three center conjugated π bonds and No-St-No conjugated π bonds were accounted for.
1992, 3(7): 563-564
Abstract:
The structure of aggregation state and isothermal crystallization behavior of Nylon-1010 have been studied by WAXD, DSC, Variance-Range Function and density measurement. The results show that crystallization of Nylon-1010 has the most suitable annealing temperature, the crystals of the Nxlon-1010 are two-dimension heterogeneous nucleation. Both low treatment temperature and high crystallization te, temperature are disadvantageous for Nylon-1010 crystal growth.
The structure of aggregation state and isothermal crystallization behavior of Nylon-1010 have been studied by WAXD, DSC, Variance-Range Function and density measurement. The results show that crystallization of Nylon-1010 has the most suitable annealing temperature, the crystals of the Nxlon-1010 are two-dimension heterogeneous nucleation. Both low treatment temperature and high crystallization te, temperature are disadvantageous for Nylon-1010 crystal growth.
1992, 3(7): 565-568
Abstract:
Covalently linked phthalocyanine complexes were incorporated in bilayer lipid membranes(BLN) and deposited on SnO2 transparent electrodes, Their photovoltages were measured and compared. It has been found that a more favorable orientation and closer proximity are attained in the diad compounds between the donor (phthalocyanine)-acceptor (anthraquinone) pair than in the simple compound for efficient light-induced charge separation and transfer. The triad compound is the best among all tested compounds.
Covalently linked phthalocyanine complexes were incorporated in bilayer lipid membranes(BLN) and deposited on SnO2 transparent electrodes, Their photovoltages were measured and compared. It has been found that a more favorable orientation and closer proximity are attained in the diad compounds between the donor (phthalocyanine)-acceptor (anthraquinone) pair than in the simple compound for efficient light-induced charge separation and transfer. The triad compound is the best among all tested compounds.
1992, 3(7): 569-572
Abstract:
The redox behaviours of the donor-acceptor model compounds, cyanoethenyl aniline derivatives were investigated by cyclic voltammetry and the mechanism of the electrode reaction was studied in detail.
The redox behaviours of the donor-acceptor model compounds, cyanoethenyl aniline derivatives were investigated by cyclic voltammetry and the mechanism of the electrode reaction was studied in detail.
1992, 3(7): 573-576
Abstract:
Highly substituted n-atkyl celluloses with sidechains 3 to 10 carbon atoms long have been prepared from cellulose acetate, sodium hydroxide and n-alkyl bromides with dimethyl sulfoxide as solvent. Synthetic conditions of n-alkyl celluloses were studied with respect to reaction temperature, time and yield. The molecular structure of the n-alkyl celluloses, which were obtained as white powders or as sticky, soft and birefringent solids at room temperature, was investigated by IR and NMR spectra and elemental analysine cholesteric phases in some non-polar solvents. The melting behavior and solubility of the n-alkyl celluloses were examined.
Highly substituted n-atkyl celluloses with sidechains 3 to 10 carbon atoms long have been prepared from cellulose acetate, sodium hydroxide and n-alkyl bromides with dimethyl sulfoxide as solvent. Synthetic conditions of n-alkyl celluloses were studied with respect to reaction temperature, time and yield. The molecular structure of the n-alkyl celluloses, which were obtained as white powders or as sticky, soft and birefringent solids at room temperature, was investigated by IR and NMR spectra and elemental analysine cholesteric phases in some non-polar solvents. The melting behavior and solubility of the n-alkyl celluloses were examined.
1992, 3(7): 577-578
Abstract:
Superconductor YBa2Cu3O7-x used as a material for lithium battery was examined in 1M LiClO4 propylene carbonate/1,2-dimethoxyethane (1:1) solution. YBa2Cu3O7-x exhibited 150 mAh/g of discharge capacity at 250 uA/cm2 discharge current. An ac impedance measurements was carried out, the results have shown that the electrode reaction has low charge-transfer resistance and the chemical diffusion coeffic ient of Li+ has a value of 10-11 cm2/sec.
Superconductor YBa2Cu3O7-x used as a material for lithium battery was examined in 1M LiClO4 propylene carbonate/1,2-dimethoxyethane (1:1) solution. YBa2Cu3O7-x exhibited 150 mAh/g of discharge capacity at 250 uA/cm2 discharge current. An ac impedance measurements was carried out, the results have shown that the electrode reaction has low charge-transfer resistance and the chemical diffusion coeffic ient of Li+ has a value of 10-11 cm2/sec.
