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1992 Volume 3 Issue 3
1992, 3(3): 157-158
Abstract:
2-Acetyl-5-methyl-2H-1,2,3-diaraphosphole 1 reacted with 2-butyne-1, 4-diol to form a tricoordinated phosphorus compound 7, which then rearranged to a novel 2, 3-disubstituted-1, 3-diene.Similar rearrangement has been observed when diphenylchloropbosphine reacted with 2-butyne-1,4-diol.
2-Acetyl-5-methyl-2H-1,2,3-diaraphosphole 1 reacted with 2-butyne-1, 4-diol to form a tricoordinated phosphorus compound 7, which then rearranged to a novel 2, 3-disubstituted-1, 3-diene.Similar rearrangement has been observed when diphenylchloropbosphine reacted with 2-butyne-1,4-diol.
1992, 3(3): 159-160
Abstract:
Michael addition of nitroalkanes to α,β-unsaturated carbonyl compounds occurs in the presence of KF/AI2O3/PEG4000 without solvent.Yields are fair to good and work-ups are easy.
Michael addition of nitroalkanes to α,β-unsaturated carbonyl compounds occurs in the presence of KF/AI2O3/PEG4000 without solvent.Yields are fair to good and work-ups are easy.
1992, 3(3): 161-162
Abstract:
This paper reports a simple method for the synthesis of amino acid ester derivatives of benzisoselenazolone.Their anticancer activity is also given.
This paper reports a simple method for the synthesis of amino acid ester derivatives of benzisoselenazolone.Their anticancer activity is also given.
1992, 3(3): 163-164
Abstract:
The acetylated xylo-and arabinopyranosyl esters (1-8) were obtained in high yields with stereoselectivity by phase-transfer catalyzed (PTC) synthesis, and their structures were confirmed by elemental analysis and IR,1H-NMR spectral data.
The acetylated xylo-and arabinopyranosyl esters (1-8) were obtained in high yields with stereoselectivity by phase-transfer catalyzed (PTC) synthesis, and their structures were confirmed by elemental analysis and IR,1H-NMR spectral data.
1992, 3(3): 165-166
Abstract:
6-O-Mcthylgossypol (3) was obtained with the methods of synthesis for the first time.
6-O-Mcthylgossypol (3) was obtained with the methods of synthesis for the first time.
1992, 3(3): 167-170
Abstract:
A series of di-n-hexyl alkyl phosphonates with bulky substituent on phosphorus was synthesized by PTC P-alkylation using crown ether.Upon saponification of the resulting di-n-hexyl alkylphosphonates in the presence of crown ether or quaternary ammonium halide, corresponding mono-hexyl esters of alkyl phosphonic acids were prepared.Ultrasonic wave, as we found, can catalyze the reaction between dialkyl phosphite & metallic sodium and hydrolysis of dihexyl alkyl phosphonates.A series of di-t-alkyl phosphinic acids were synthesized by the reaction of Grignard reagent with PCl3 followed by oxidation with 30% H2O2.It was found that the reaction between dibutyl phosphite and Grignard reagent of t-alkyl chloride is a new synthetic method for the preparation of mono-esters of highly hindered alkyl phosphonic acids.
A series of di-n-hexyl alkyl phosphonates with bulky substituent on phosphorus was synthesized by PTC P-alkylation using crown ether.Upon saponification of the resulting di-n-hexyl alkylphosphonates in the presence of crown ether or quaternary ammonium halide, corresponding mono-hexyl esters of alkyl phosphonic acids were prepared.Ultrasonic wave, as we found, can catalyze the reaction between dialkyl phosphite & metallic sodium and hydrolysis of dihexyl alkyl phosphonates.A series of di-t-alkyl phosphinic acids were synthesized by the reaction of Grignard reagent with PCl3 followed by oxidation with 30% H2O2.It was found that the reaction between dibutyl phosphite and Grignard reagent of t-alkyl chloride is a new synthetic method for the preparation of mono-esters of highly hindered alkyl phosphonic acids.
1992, 3(3): 171-172
Abstract:
The products of basic hydrolysis of ethyl oxal-acetate and the preparation of 3-ethoxy carbonyl pyruvic acid 1 are reported.Esterification reaction of 1 with unhindered alcohols could be carried out smoothly, but it was unsuccessful with hindered alcohols.
The products of basic hydrolysis of ethyl oxal-acetate and the preparation of 3-ethoxy carbonyl pyruvic acid 1 are reported.Esterification reaction of 1 with unhindered alcohols could be carried out smoothly, but it was unsuccessful with hindered alcohols.
1992, 3(3): 173-174
Abstract:
The chiral oxiranecarboxylic acids or esters 2a-e were obtained with lipase (CCL) in aqueous-organic system.The ee and the absolute configurations of the products were determined.
The chiral oxiranecarboxylic acids or esters 2a-e were obtained with lipase (CCL) in aqueous-organic system.The ee and the absolute configurations of the products were determined.
1992, 3(3): 175-176
Abstract:
Acylation of 5-methyl-3-hydroxyisoxazole (1) with 3-substituted cyclopropanecarboxylic chlorides (3) in the presence of triethylamine (TEA) in acetonitrile yields predominantly O-acylated products (4).The N-acyl isomers (5) are afforded regiospecifically using trimethylsilyl ether of 3-hydroxyisoxazole (2).
Acylation of 5-methyl-3-hydroxyisoxazole (1) with 3-substituted cyclopropanecarboxylic chlorides (3) in the presence of triethylamine (TEA) in acetonitrile yields predominantly O-acylated products (4).The N-acyl isomers (5) are afforded regiospecifically using trimethylsilyl ether of 3-hydroxyisoxazole (2).
1992, 3(3): 177-178
Abstract:
A new synthetic route to α-damascone (4) starting from citral is described-The synthesis features allylatioa of α-cyclocitral (1) with allylic bromide in the presence of tin powder to give the crucial intermediate 1-(2',6',6'-trimethylcyclo-hexen-2'-yl)-3-buten-1-ol (2a) and (2b) in a combined yield of 70%.
A new synthetic route to α-damascone (4) starting from citral is described-The synthesis features allylatioa of α-cyclocitral (1) with allylic bromide in the presence of tin powder to give the crucial intermediate 1-(2',6',6'-trimethylcyclo-hexen-2'-yl)-3-buten-1-ol (2a) and (2b) in a combined yield of 70%.
1992, 3(3): 179-180
Abstract:
Three kinds of products have been separated from the reaction mixtures of 1,2-dihydro-2, 4-disubstituted-1,5-benzodiazepine with:CCI2.Besides the addition products of:CCI2 to C=N.the inserted products of:CCI2 to N-H and C-H single bonds were obtained, too.
Three kinds of products have been separated from the reaction mixtures of 1,2-dihydro-2, 4-disubstituted-1,5-benzodiazepine with:CCI2.Besides the addition products of:CCI2 to C=N.the inserted products of:CCI2 to N-H and C-H single bonds were obtained, too.
1992, 3(3): 181-182
Abstract:
Addition of a-carbonylketenes, generated from 2-diazo-1, 3-diaryl-1, 3-propandione or 2-diazo-1-phenyl-1,3-butandione by heating, to 2,4-diaryl-2,3-dihydro-[1,5]-benzothiazepines gave 2,3-disubstituted-4a, 6-diaryl-4a,5,6,12-telrahydro-1H-1, 3-oxazino[3,2d] [1,5]-benzothiazepine-l-ones, a new ring system.
Addition of a-carbonylketenes, generated from 2-diazo-1, 3-diaryl-1, 3-propandione or 2-diazo-1-phenyl-1,3-butandione by heating, to 2,4-diaryl-2,3-dihydro-[1,5]-benzothiazepines gave 2,3-disubstituted-4a, 6-diaryl-4a,5,6,12-telrahydro-1H-1, 3-oxazino[3,2d] [1,5]-benzothiazepine-l-ones, a new ring system.
1992, 3(3): 183-184
Abstract:
α-Acetamidocinnamamide do not react with P(OMe)3, with P(NEt2)3 they give rise to 2-methyl-4-hydroxy-5-α-[bis (diethylamino) phosphoryl] benzyl imidazole.The pathway is studied for the formation of Ⅰ. The two intermediates(Ⅱ) are isolated.The structures of Ⅰ and Ⅱ are confirmed by IR, 1H NMR, 31P NMR, Ms.
α-Acetamidocinnamamide do not react with P(OMe)3, with P(NEt2)3 they give rise to 2-methyl-4-hydroxy-5-α-[bis (diethylamino) phosphoryl] benzyl imidazole.The pathway is studied for the formation of Ⅰ. The two intermediates(Ⅱ) are isolated.The structures of Ⅰ and Ⅱ are confirmed by IR, 1H NMR, 31P NMR, Ms.
1992, 3(3): 185-188
Abstract:
New clerodane diterpenoids-tinocallone A, B, C, D and epitinopaylloloside (1-4.and 8) have been isolated from the root of Tinospora capillipes.Their structures were elucidated by chemical and spectral analysis.
New clerodane diterpenoids-tinocallone A, B, C, D and epitinopaylloloside (1-4.and 8) have been isolated from the root of Tinospora capillipes.Their structures were elucidated by chemical and spectral analysis.
1992, 3(3): 189-190
Abstract:
Three flavonoids have been isolated from the leaves of Glycyrrhiza uralensis Fisch (licorice,Leguminosae).The structures have been identified as 5,7,3',4'-tetrahydroxy-3-methoxy-5'-isoprenyl flavone (I,uralenol-3-methylether),5,6,3',4'-tetrahydroxy-3-methoxy-6'-isoprenyl flavone (Ⅱ, unalene) and quercetin (Ⅲ).Ⅰ and Ⅱ are new compound.
Three flavonoids have been isolated from the leaves of Glycyrrhiza uralensis Fisch (licorice,Leguminosae).The structures have been identified as 5,7,3',4'-tetrahydroxy-3-methoxy-5'-isoprenyl flavone (I,uralenol-3-methylether),5,6,3',4'-tetrahydroxy-3-methoxy-6'-isoprenyl flavone (Ⅱ, unalene) and quercetin (Ⅲ).Ⅰ and Ⅱ are new compound.
1992, 3(3): 191-192
Abstract:
The equation derived for the response of the current transients in the flowing fluid is verified experimentally.
The equation derived for the response of the current transients in the flowing fluid is verified experimentally.
1992, 3(3): 193-196
Abstract:
A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.
A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.
1992, 3(3): 197-200
Abstract:
This paper describes a simple method for the preparation of L-proline stationary phase bonded to silica gel and characterization of the bonded phase by IR spectrometry, elemental analysis and nitrogen adsorption method at low temperature.The enantiomeric resolutions of 3-(2-pyridyl)-3-aminopropionic acid and 2,3-diaminobutanoic acid on the bonded phase were carried out.
This paper describes a simple method for the preparation of L-proline stationary phase bonded to silica gel and characterization of the bonded phase by IR spectrometry, elemental analysis and nitrogen adsorption method at low temperature.The enantiomeric resolutions of 3-(2-pyridyl)-3-aminopropionic acid and 2,3-diaminobutanoic acid on the bonded phase were carried out.
1992, 3(3): 201-204
Abstract:
1,10-phenanthroline and its derivatives can form charge-transfer complexes with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ).The absorption spectra and conditions of complex formation,such as the reaction time,the quantity of DDQ, and the solvents, have been studied.After the HMO calculation of phenanthrolines,the molar absorptivities were found to depend on the substituents on the phenanthroline rings.
1,10-phenanthroline and its derivatives can form charge-transfer complexes with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ).The absorption spectra and conditions of complex formation,such as the reaction time,the quantity of DDQ, and the solvents, have been studied.After the HMO calculation of phenanthrolines,the molar absorptivities were found to depend on the substituents on the phenanthroline rings.
1992, 3(3): 205-206
Abstract:
Theories of the second reciprocal derivative chronopotentiometry analysis were deduced and experimentally verificated.Results in this study show that chronopotentiometry is significantly developed in both sensitivity and resolution for signals treated by the second reciprocal derivative.
Theories of the second reciprocal derivative chronopotentiometry analysis were deduced and experimentally verificated.Results in this study show that chronopotentiometry is significantly developed in both sensitivity and resolution for signals treated by the second reciprocal derivative.
1992, 3(3): 207-210
Abstract:
Thermotropic liquid crystalline VHE terpolyesters made from vanillic acid (V),p-hydroxybenzoic acid (H) and poly (ethylene terephthalate) (E) were studied by 400 MHz NMR spectra, wide angle X-ray diffraction,scanning electron and polarizing microscopes.It was found that the VHE terpolyesters had random sequence distribution.The VHE terpolyester films exhibited highly oriented fibrillar structure.
Thermotropic liquid crystalline VHE terpolyesters made from vanillic acid (V),p-hydroxybenzoic acid (H) and poly (ethylene terephthalate) (E) were studied by 400 MHz NMR spectra, wide angle X-ray diffraction,scanning electron and polarizing microscopes.It was found that the VHE terpolyesters had random sequence distribution.The VHE terpolyester films exhibited highly oriented fibrillar structure.
1992, 3(3): 211-212
Abstract:
The crystal structure of Di-nitratobis (ethylcaprolactam)uranyl (Ⅱ) UO2 [CH2 (CH2)4 CONC2H5]2 (NO3)2 was established by a single-crystal X-ray diffraction study.It is triclinie, space group P1, with a=7.171 (2), b=8.655 (3), c=10.182 (5)Å, α=78.27 (3), β=70.63 (3), γ=81.76 (3)°, V=581.7 (4)Å3, Z=l, Dc=1.94 g.cm-3.Final R value is 0.0218.The result reveals that uranyl ion is coordinated to six oxygen atoms, two of them are from two carbonyl groups of ethylcaprolactam and the other four are from two nitrate groups.
The crystal structure of Di-nitratobis (ethylcaprolactam)uranyl (Ⅱ) UO2 [CH2 (CH2)4 CONC2H5]2 (NO3)2 was established by a single-crystal X-ray diffraction study.It is triclinie, space group P1, with a=7.171 (2), b=8.655 (3), c=10.182 (5)Å, α=78.27 (3), β=70.63 (3), γ=81.76 (3)°, V=581.7 (4)Å3, Z=l, Dc=1.94 g.cm-3.Final R value is 0.0218.The result reveals that uranyl ion is coordinated to six oxygen atoms, two of them are from two carbonyl groups of ethylcaprolactam and the other four are from two nitrate groups.
1992, 3(3): 213-214
Abstract:
Synthetic goethite (α-FeOOH) was prepared in the laboratory using a modified version of Brauer's method[1].The process of steam-crystallization was prolonged and impurities were removed by dialysis.The products have been characterised by Surface Area Analyser and Scanning Electron Microscope, and proved to have larger Specific Surface Area than that in literature.
Synthetic goethite (α-FeOOH) was prepared in the laboratory using a modified version of Brauer's method[1].The process of steam-crystallization was prolonged and impurities were removed by dialysis.The products have been characterised by Surface Area Analyser and Scanning Electron Microscope, and proved to have larger Specific Surface Area than that in literature.
1992, 3(3): 215-216
Abstract:
Electrochemical Betted not only can obtain the conducting film of polyaniline on a glass carbon electrode, but also can imobilize PMo12O403- in the film to form a organic conducting film electrode modified by heteropolyanion.The paper here reports electrochemical changes in the preparation of PMo12O403--polyaniline modified electrode, the electrochemical reaction mechanism of the modified electrode was obtained from the study on its redox properties.Moreover, the above electrode showed marked electrocatalysis for the reduction reaction of CIO3-.
Electrochemical Betted not only can obtain the conducting film of polyaniline on a glass carbon electrode, but also can imobilize PMo12O403- in the film to form a organic conducting film electrode modified by heteropolyanion.The paper here reports electrochemical changes in the preparation of PMo12O403--polyaniline modified electrode, the electrochemical reaction mechanism of the modified electrode was obtained from the study on its redox properties.Moreover, the above electrode showed marked electrocatalysis for the reduction reaction of CIO3-.
1992, 3(3): 217-218
Abstract:
Under steady-state conditions, the general currents of EE reactions at disk,hemispherical and spherical microelectrodes are derived.From these equations, some electrode reaction parameters can be very simply obtained.
Under steady-state conditions, the general currents of EE reactions at disk,hemispherical and spherical microelectrodes are derived.From these equations, some electrode reaction parameters can be very simply obtained.
1992, 3(3): 219-222
Abstract:
Phase sepertion of 9-cis-retinal schiff base in two-component LB film with different lipids has been observed under Brewster Angle Microscope.
Phase sepertion of 9-cis-retinal schiff base in two-component LB film with different lipids has been observed under Brewster Angle Microscope.
1992, 3(3): 223-226
Abstract:
The photocatalytic decomposition of methanol in the presence of vanadium dichloride and the transfer of hydrogen and methyl free radicals to the additives and dinitrogen were reported.
The photocatalytic decomposition of methanol in the presence of vanadium dichloride and the transfer of hydrogen and methyl free radicals to the additives and dinitrogen were reported.
1992, 3(3): 227-230
Abstract:
The structures and catalytic performances of V2O5, Mg3V2O8 and V/MgO catalysts have been correlated by means of XRD, FTIR, TPR and flow micro-reactor tests. The postulation about active site has been made. Based on it, better catalysts have been first prepared via grafting and modification with Sb which are better than that via impregnation.
The structures and catalytic performances of V2O5, Mg3V2O8 and V/MgO catalysts have been correlated by means of XRD, FTIR, TPR and flow micro-reactor tests. The postulation about active site has been made. Based on it, better catalysts have been first prepared via grafting and modification with Sb which are better than that via impregnation.
1992, 3(3): 231-234
Abstract:
The coaggregating behavior of the cationic kinetic probe P16+ with different types of surfactants are in complete agreement with predictions based on the newly proposed ESAg concept.
The coaggregating behavior of the cationic kinetic probe P16+ with different types of surfactants are in complete agreement with predictions based on the newly proposed ESAg concept.
