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1995 Volume 6 Issue 10
1995, 6(10): 833-834
Abstract:
Pyridine and 4-picoline undergo reductive tetraallylation with allyl bromide and zinc dust in THF at room temperature to afford regio-selectively 1,2,3,6-tetraallyl-1,2,3,6-tetrahydropyridine and 1,2,3,6-tetraallyl-1,2,3,6-tetrahydro-4-picoline, respectively.
Pyridine and 4-picoline undergo reductive tetraallylation with allyl bromide and zinc dust in THF at room temperature to afford regio-selectively 1,2,3,6-tetraallyl-1,2,3,6-tetrahydropyridine and 1,2,3,6-tetraallyl-1,2,3,6-tetrahydro-4-picoline, respectively.
1995, 6(10): 835-838
Abstract:
The discovery of a rearrangement reaction of 5-amino-1-arylaminocarbcnyl-1,2,4-triazole (pyrazole) to 5-arylureylene-1,2,4-trazole and the mechanism for this rearrangement reaction are presented.The rearrangement reaction could be attributed to a thermodynamic energy preference leading to the predominant formation of 5-arylureylene-1,2,4-triazole,as shown by molecular mechanics calculation with MMX program.
The discovery of a rearrangement reaction of 5-amino-1-arylaminocarbcnyl-1,2,4-triazole (pyrazole) to 5-arylureylene-1,2,4-trazole and the mechanism for this rearrangement reaction are presented.The rearrangement reaction could be attributed to a thermodynamic energy preference leading to the predominant formation of 5-arylureylene-1,2,4-triazole,as shown by molecular mechanics calculation with MMX program.
1995, 6(10): 839-842
Abstract:
In the presence of reactive alkali metal hydrides,nitriles can be cyclotrimerized to give 2,4,6-trisubstituted-1,3,5-triazines and 2,4,6-trisubstituted imidazoles in moderate yield.
In the presence of reactive alkali metal hydrides,nitriles can be cyclotrimerized to give 2,4,6-trisubstituted-1,3,5-triazines and 2,4,6-trisubstituted imidazoles in moderate yield.
1995, 6(10): 843-846
Abstract:
Nine 2-aryl-4-phenyloxazoles are prepared from phenacyl benzoates and acetamide in boiling xylene under the action of boron fluoride as catalyst.By this improved method the oxazoles are obtained as single products with yields ranging 75-90%.
Nine 2-aryl-4-phenyloxazoles are prepared from phenacyl benzoates and acetamide in boiling xylene under the action of boron fluoride as catalyst.By this improved method the oxazoles are obtained as single products with yields ranging 75-90%.
1995, 6(10): 847-850
Abstract:
In search for anticancer agents,thirteen new α,β-unsaturated and β-aminomethyl cyclopentanones containing α-(1-cyclopentenyl) have been synthesized by condensation and by Mannich reaction respectively.Anticancer test showed that all title compounds have significant activities against P385,Hela.HepA and EAC in vitro.Part of these compounds were shown to have activity against EAC tumour in vivo.
In search for anticancer agents,thirteen new α,β-unsaturated and β-aminomethyl cyclopentanones containing α-(1-cyclopentenyl) have been synthesized by condensation and by Mannich reaction respectively.Anticancer test showed that all title compounds have significant activities against P385,Hela.HepA and EAC in vitro.Part of these compounds were shown to have activity against EAC tumour in vivo.
1995, 6(10): 851-852
Abstract:
Using cation exchange resin (D72,Amberlyst-15) as catalyst,Mannich-type reaction of 5-amino-1,2,4-triazole 1,containing guanidine substructure,provides an efficient synthesis of a new kind of bicyclic P-and N-containing compounds,6-phospha-4,5,6-trihydroimidazolo [2,3-e] 1,2,4-triazofe 4.
Using cation exchange resin (D72,Amberlyst-15) as catalyst,Mannich-type reaction of 5-amino-1,2,4-triazole 1,containing guanidine substructure,provides an efficient synthesis of a new kind of bicyclic P-and N-containing compounds,6-phospha-4,5,6-trihydroimidazolo [2,3-e] 1,2,4-triazofe 4.
1995, 6(10): 853-854
Abstract:
3',4'-Methylenedioxyisodericine-A and pongapinone-B were first synthesized via the condensation of piperonal with 2-hydroxy-4-methoxy-3-prenylacetophenone and 4,6-dimethoxy-2-hydroxy-3-prenylacetophenone respectively followed by cyclization.
3',4'-Methylenedioxyisodericine-A and pongapinone-B were first synthesized via the condensation of piperonal with 2-hydroxy-4-methoxy-3-prenylacetophenone and 4,6-dimethoxy-2-hydroxy-3-prenylacetophenone respectively followed by cyclization.
1995, 6(10): 855-856
Abstract:
The spirobicyclic pentacoordinated germanium compounds are synthesized by one pot reaction of diethyl N,N-bis-(2-hydroxyethyl) aminomethyl phosphonate with tetraethoxygermane and Z(OH)2(Z=CH2CH2,CH(CH3)CH2,CH(CH3)CH(CH3),1,2-C6H4).The products were confirmed by 1HNMR,31PNMR and MS spectra.
The spirobicyclic pentacoordinated germanium compounds are synthesized by one pot reaction of diethyl N,N-bis-(2-hydroxyethyl) aminomethyl phosphonate with tetraethoxygermane and Z(OH)2(Z=CH2CH2,CH(CH3)CH2,CH(CH3)CH(CH3),1,2-C6H4).The products were confirmed by 1HNMR,31PNMR and MS spectra.
1995, 6(10): 857-860
Abstract:
This paper describes a facile synthesis of chiral 3-alkyl-3,4-dihydro-2H-1,4-benzoxazine derivatives 1,in which (S) or (R) configuration (1b or 1c)is obtainable.
This paper describes a facile synthesis of chiral 3-alkyl-3,4-dihydro-2H-1,4-benzoxazine derivatives 1,in which (S) or (R) configuration (1b or 1c)is obtainable.
1995, 6(10): 861-862
Abstract:
Two kinds of phosphono-dipeptides have been synthesized by the Mannich-type or Arbuzov-type reaction.The structures of new products have been confirmed by 1H NMR,31P NMR,IR,MS and elemental analyses.
Two kinds of phosphono-dipeptides have been synthesized by the Mannich-type or Arbuzov-type reaction.The structures of new products have been confirmed by 1H NMR,31P NMR,IR,MS and elemental analyses.
1995, 6(10): 863-866
Abstract:
A polyunsaturated mixed-acid phosphatidylcholine, 1-palmitoyl-2-linoienoyl-sn-glycerophosphocholine (1) prepared from D-mannitol as an optically active starting material is described.
A polyunsaturated mixed-acid phosphatidylcholine, 1-palmitoyl-2-linoienoyl-sn-glycerophosphocholine (1) prepared from D-mannitol as an optically active starting material is described.
1995, 6(10): 867-870
Abstract:
The interaction between C60 cage and the center halogen atoms in endohedral complexes (Halogen@C60) (Halogen=Hal=F,Cl,Br,I),including electro-static interaction,dispersive interaction and repulsive interaction,have been calculated by molecular mechanics method combined with the results obtained by quantum-chemical EHMO/ASED method.The computational results show that the total interaction is attraction which reduces the energy of the endohedral complex system except for (I@C60),and the electro-static interaction plays a decisive role in the three forms of interactions,reaching up more than 90%.For the endohedral complex (I@C60),the resultant non-bonded interaction is repulsive.There is a similar variation trend for the total energy variation of system △Etot and the total interaction energy Einter,of which the order is (F@C60) < (Cl@C60) < (Br@C60) < (I@C60).
The interaction between C60 cage and the center halogen atoms in endohedral complexes (Halogen@C60) (Halogen=Hal=F,Cl,Br,I),including electro-static interaction,dispersive interaction and repulsive interaction,have been calculated by molecular mechanics method combined with the results obtained by quantum-chemical EHMO/ASED method.The computational results show that the total interaction is attraction which reduces the energy of the endohedral complex system except for (I@C60),and the electro-static interaction plays a decisive role in the three forms of interactions,reaching up more than 90%.For the endohedral complex (I@C60),the resultant non-bonded interaction is repulsive.There is a similar variation trend for the total energy variation of system △Etot and the total interaction energy Einter,of which the order is (F@C60) < (Cl@C60) < (Br@C60) < (I@C60).
A NEW APPLICATION OF HYDRIZIRCONOCENE CHLORIDE,CROSS COUPLING OF ALKENYL STANNANE WITH ALLYL BROMIDE
1995, 6(10): 871-872
Abstract:
Alkenyl stannane after hydrozirconation,coupled with allyl bromide using CuCN as catalyst producing allyl homologated stannane.
Alkenyl stannane after hydrozirconation,coupled with allyl bromide using CuCN as catalyst producing allyl homologated stannane.
1995, 6(10): 873-874
Abstract:
A new triterpene alcohol was isolated and identifed by specrtral analyses from Skimmia laureola ssp.multinervia which was collected from Yunnan province of China and named O-methyllaureolol.
A new triterpene alcohol was isolated and identifed by specrtral analyses from Skimmia laureola ssp.multinervia which was collected from Yunnan province of China and named O-methyllaureolol.
1995, 6(10): 875-876
Abstract:
A new eremophilane acid was isolated in the phytochemical investigation of the roots of Ligularia sagitta.Its structure and stereochemistry were elucidated by 1D NMR and 2D NMR techniques including 1H-1H COSY,13C-1H COSY,13C-1H COLOC and NOESY.
A new eremophilane acid was isolated in the phytochemical investigation of the roots of Ligularia sagitta.Its structure and stereochemistry were elucidated by 1D NMR and 2D NMR techniques including 1H-1H COSY,13C-1H COSY,13C-1H COLOC and NOESY.
1995, 6(10): 877-878
Abstract:
A new quinolone alkaloid was isolated from the fruit of Evodia rutaecarpa Bentham (Rutaceae) with three known alkaloids,and their structures were determined on the basis of spectral data and chemical transformations.
A new quinolone alkaloid was isolated from the fruit of Evodia rutaecarpa Bentham (Rutaceae) with three known alkaloids,and their structures were determined on the basis of spectral data and chemical transformations.
1995, 6(10): 879-882
Abstract:
In this paper,the interaction of tripositive terbium ions (Tb3+) with bovine serum albumin (DSA) has been investigated in the presence of some alkaline earth metals and citric acid (Cit) by using fluorescence spectroscopy.The results show that Tb3+,BSA and Cit can form ternary complex BSA·Tb2·Cit4 in μ=0.1mol/1 NaCl,pH 6.3 hexaniethylenetetramine buffer.Other rare earths are able to compete for the same binding site in BSA with Tb3+.The sequence of competition is Eu3+ > Pr3+ > Yb3+ > Gd3+ > La3+.Ca2+ and Mg2+ can not replace Tb bound to BSA.
In this paper,the interaction of tripositive terbium ions (Tb3+) with bovine serum albumin (DSA) has been investigated in the presence of some alkaline earth metals and citric acid (Cit) by using fluorescence spectroscopy.The results show that Tb3+,BSA and Cit can form ternary complex BSA·Tb2·Cit4 in μ=0.1mol/1 NaCl,pH 6.3 hexaniethylenetetramine buffer.Other rare earths are able to compete for the same binding site in BSA with Tb3+.The sequence of competition is Eu3+ > Pr3+ > Yb3+ > Gd3+ > La3+.Ca2+ and Mg2+ can not replace Tb bound to BSA.
1995, 6(10): 883-884
Abstract:
The binding of coordination compound Ru(phen)32+ to calf thymus DMA and herring sperm DNA has been investigated by absorption,emission and circular dichroism spectroscopy. Measurement of enantioselectivily combined with photophysical experiment shows the binding of Ru(phen)32+ with calf thymus DNA is of intercalatively bound mode,but the binding of Ru(phen)32+ with herring sperm DNA is of surface-bound mode.
The binding of coordination compound Ru(phen)32+ to calf thymus DMA and herring sperm DNA has been investigated by absorption,emission and circular dichroism spectroscopy. Measurement of enantioselectivily combined with photophysical experiment shows the binding of Ru(phen)32+ with calf thymus DNA is of intercalatively bound mode,but the binding of Ru(phen)32+ with herring sperm DNA is of surface-bound mode.
1995, 6(10): 885-886
Abstract:
UV and Raman spectra were used in the studies of anionic species in sodium aluminate solutions.Two absorption peaks near 233nm and 270nm in UV spectra were found and assigned to Al(OH)4 and [(HO)3Al-O-Al(OH)3]2- respectively,while the results of Raman spectra measurements and quantum chemical calculations by using MNDO and DV-Xα methods were in good agreement with the above conclusions.
UV and Raman spectra were used in the studies of anionic species in sodium aluminate solutions.Two absorption peaks near 233nm and 270nm in UV spectra were found and assigned to Al(OH)4 and [(HO)3Al-O-Al(OH)3]2- respectively,while the results of Raman spectra measurements and quantum chemical calculations by using MNDO and DV-Xα methods were in good agreement with the above conclusions.
1995, 6(10): 887-890
Abstract:
The bonding mechanisms between the first-row transition metal and carbon monoxide were discussed.Three basic rules have been drawn up to determine the ground states of the metal monocarbonyls.The theoretical assignments are in full agreement with the existing experimental results.
The bonding mechanisms between the first-row transition metal and carbon monoxide were discussed.Three basic rules have been drawn up to determine the ground states of the metal monocarbonyls.The theoretical assignments are in full agreement with the existing experimental results.
1995, 6(10): 891-892
Abstract:
Two new ligands.aroyl hydrazones containing triazole and some of their bivalent transition metal complexes have been synthesized.The complexes were characterized by elemental analyses,IR,UV,XPS and thermal analyses.Two ligands were characterized by NMR spectra also.
Two new ligands.aroyl hydrazones containing triazole and some of their bivalent transition metal complexes have been synthesized.The complexes were characterized by elemental analyses,IR,UV,XPS and thermal analyses.Two ligands were characterized by NMR spectra also.
1995, 6(10): 893-896
Abstract:
Two new polypyridine liganda,imidazo[f]1,10-phenanthroline (IP) and 2-phenyl-imidazo[f]1,10-phenanthroline (PIP) and their Ru(Ⅱ) mixed type coordination compounds together with 2,2'-bipyridine (bpy) and 1,10-phenanthroline(phen) are synthesized and characterized by elemental analyses,melting points,electronic absorption,IR,emission spectra and cyclic voltammetry.
Two new polypyridine liganda,imidazo[f]1,10-phenanthroline (IP) and 2-phenyl-imidazo[f]1,10-phenanthroline (PIP) and their Ru(Ⅱ) mixed type coordination compounds together with 2,2'-bipyridine (bpy) and 1,10-phenanthroline(phen) are synthesized and characterized by elemental analyses,melting points,electronic absorption,IR,emission spectra and cyclic voltammetry.
1995, 6(10): 897-898
Abstract:
The title compound (Me2SiSiMe2)[η5-1-indenyl)Fe(CO)]2(μ-CO)2(1) was prepared by the reaction of 1.2-bis(1-indenyl)tetramethyldisilane and Fe(CO)5 in relluxing heptane.1 in refluxing xylene can be converted into [Me2Si(η5-1-indenyl) Fe(CO)2]2(2).The pure trans isomer 2t was obtained and its crystal and molecular structure was determined by X-ray diffraction.
The title compound (Me2SiSiMe2)[η5-1-indenyl)Fe(CO)]2(μ-CO)2(1) was prepared by the reaction of 1.2-bis(1-indenyl)tetramethyldisilane and Fe(CO)5 in relluxing heptane.1 in refluxing xylene can be converted into [Me2Si(η5-1-indenyl) Fe(CO)2]2(2).The pure trans isomer 2t was obtained and its crystal and molecular structure was determined by X-ray diffraction.
1995, 6(10): 899-902
Abstract:
(Et4N)2Pd(i-mnt)2,fw=647.04,monociinic,space group P21/c;a=9.511(1),b=11.612(2),c=14.820(3)Å,β=94.38(1)°, V=1631.9(5)Å3, Z=2, Dc=1.32 g·cm-3, F(000)=672, R=0.0324, RW=0.0298. This is a new example of X-ray characterized Pd complexes with bivalent anion 1,1-dithiolato ligands and its reaction with(Et4N)2WS4 gives (Et4N)2WS4Pd(i-mnt).
(Et4N)2Pd(i-mnt)2,fw=647.04,monociinic,space group P21/c;a=9.511(1),b=11.612(2),c=14.820(3)Å,β=94.38(1)°, V=1631.9(5)Å3, Z=2, Dc=1.32 g·cm-3, F(000)=672, R=0.0324, RW=0.0298. This is a new example of X-ray characterized Pd complexes with bivalent anion 1,1-dithiolato ligands and its reaction with(Et4N)2WS4 gives (Et4N)2WS4Pd(i-mnt).
1995, 6(10): 903-906
Abstract:
Two strong fluorescent amphiphilic europium-dibenzoylmethane complex:Me3NC16H33.Fu(DBM)4.(A) and Et3NC18H37.Eu(DBM)4 (B) have been synthesized and their Langmuir films have been formed at the air/water interface.The Langmuir film of A can be easily transferred onto hydrophilic substrates with transfer ratio around unity to build up Langmuir-Blodgett (LB) films.The LB films were characterized by UV-vis spectra and low-angle X-ray diffraction.Their fluorescence spectra and fluorescence lifetime have been studied both in solution and highly ordered LB films.
Two strong fluorescent amphiphilic europium-dibenzoylmethane complex:Me3NC16H33.Fu(DBM)4.(A) and Et3NC18H37.Eu(DBM)4 (B) have been synthesized and their Langmuir films have been formed at the air/water interface.The Langmuir film of A can be easily transferred onto hydrophilic substrates with transfer ratio around unity to build up Langmuir-Blodgett (LB) films.The LB films were characterized by UV-vis spectra and low-angle X-ray diffraction.Their fluorescence spectra and fluorescence lifetime have been studied both in solution and highly ordered LB films.
1995, 6(10): 907-910
Abstract:
Transformation of living ring-opening metathesis polymerization (ROMP) into coordination polymerization by converting the titanacyclobutane attached to a polynorbornene (polyNBE) chain into titanocene alkoxide has been used to the synthesis of poly(NBE-b-ethylene).The copolymerization product,after being extracted by CH2Cl2 to separate the NBE homopolymer,exhibits the Tg of polyNBE segments and Tm of polyethylene segments by DSC measurement.
Transformation of living ring-opening metathesis polymerization (ROMP) into coordination polymerization by converting the titanacyclobutane attached to a polynorbornene (polyNBE) chain into titanocene alkoxide has been used to the synthesis of poly(NBE-b-ethylene).The copolymerization product,after being extracted by CH2Cl2 to separate the NBE homopolymer,exhibits the Tg of polyNBE segments and Tm of polyethylene segments by DSC measurement.
1995, 6(10): 911-914
Abstract:
FeY zeolites were prepared by three different secondary synthetic methods.Samples were characterized with XRD,IR,ESR,MBS and XPS techniques.The results showed that more iron ions were inserted into the framework of zeolite when the sample was pretreated with (NH4)2SiF6 aqueous sotution.The structure of such zeolites has obviously changed due to the iron ions inserted into the framework.
FeY zeolites were prepared by three different secondary synthetic methods.Samples were characterized with XRD,IR,ESR,MBS and XPS techniques.The results showed that more iron ions were inserted into the framework of zeolite when the sample was pretreated with (NH4)2SiF6 aqueous sotution.The structure of such zeolites has obviously changed due to the iron ions inserted into the framework.
1995, 6(10): 915-918
Abstract:
Spherical,monodispersed europium hydroxycarbonate particles were obtained by homogeneous precipitation with urea in aqueous solution of Eu(NO3)3 at elevated temperature.The particles were readily converted to the uniform EU2O3 with average particle size of 50nm after calcined at 750℃.
Spherical,monodispersed europium hydroxycarbonate particles were obtained by homogeneous precipitation with urea in aqueous solution of Eu(NO3)3 at elevated temperature.The particles were readily converted to the uniform EU2O3 with average particle size of 50nm after calcined at 750℃.
1995, 6(10): 919-922
Abstract:
Endotoxin was removed by membrane affinity chromatography.Macropore cellulose membrane was prepared from filter paper by alkaline treatment and chemical crosslinking,and was used as stationary phase for affinity chromatography.The matrix membrane was derived by hexamethylenediamine and activated by glutaraldehyde before histidine was immobilized as affinity ligand.A membrane cartridge containing 40 sheets of affinity membrane was also prepared,which can be used to remove pyrogen from aqueous solutions.
Endotoxin was removed by membrane affinity chromatography.Macropore cellulose membrane was prepared from filter paper by alkaline treatment and chemical crosslinking,and was used as stationary phase for affinity chromatography.The matrix membrane was derived by hexamethylenediamine and activated by glutaraldehyde before histidine was immobilized as affinity ligand.A membrane cartridge containing 40 sheets of affinity membrane was also prepared,which can be used to remove pyrogen from aqueous solutions.
1995, 6(10): 923-926
Abstract:
Low molecular weight materials contained in PPS resin were obtained by extracting PPS powder exhaustively with xylene and examined by solid probe mass spectroscopy.Six families of oligomers have been identified in the extract.Cyclopenta (p-phenylene sulfide) (Ⅰ) and cyclohexa (p-phenylene sulfide) (Ⅱ) have been isolated from PPS by extraction and recrystallization,and characterized.
Low molecular weight materials contained in PPS resin were obtained by extracting PPS powder exhaustively with xylene and examined by solid probe mass spectroscopy.Six families of oligomers have been identified in the extract.Cyclopenta (p-phenylene sulfide) (Ⅰ) and cyclohexa (p-phenylene sulfide) (Ⅱ) have been isolated from PPS by extraction and recrystallization,and characterized.
