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2003 Volume 14 Issue 3
2003, 14(3): 221-224
Abstract:
Piperonyl methyl ketone was obtained by oxidizing isosafrole with hydrogen peroxide and formic acid. Dianion of ethyl acetoacetate reacted with piperonyl methyl ketone and 5, 6-dihydro-6-methyl-6-piperonyl-2H-pyran-2, 4-dione was prepared, which reacted with substituted anilines in the presence of ethyl orthoformate to obtain 3-anilinomethylene-5, 6-dihydro-6-methyl-6-piperonyl-2H-pyran-2, 4-diones. Their structures were confirmed by 1HNMR and elemental analysis.
Piperonyl methyl ketone was obtained by oxidizing isosafrole with hydrogen peroxide and formic acid. Dianion of ethyl acetoacetate reacted with piperonyl methyl ketone and 5, 6-dihydro-6-methyl-6-piperonyl-2H-pyran-2, 4-dione was prepared, which reacted with substituted anilines in the presence of ethyl orthoformate to obtain 3-anilinomethylene-5, 6-dihydro-6-methyl-6-piperonyl-2H-pyran-2, 4-diones. Their structures were confirmed by 1HNMR and elemental analysis.
2003, 14(3): 225-228
Abstract:
Efficient Mukaiyama-type aldol reaction of 1, 2-bis(trimethylsiloxy)cyclobutene with aromatic aldehydes catalyzed by MgI2 is reported. The resulting succinoylation product of aldehyde was converted into the synthetic useful γ-lactone and butenolide derivatives.
Efficient Mukaiyama-type aldol reaction of 1, 2-bis(trimethylsiloxy)cyclobutene with aromatic aldehydes catalyzed by MgI2 is reported. The resulting succinoylation product of aldehyde was converted into the synthetic useful γ-lactone and butenolide derivatives.
2003, 14(3): 229-232
Abstract:
A facile glycosylation for the synthesis of spirostanol glycosides was reported. Using cadmium carbonate as a catalyst in CH3CN, a series of saponins was synthesized efficiently in a satisfactory yield.
A facile glycosylation for the synthesis of spirostanol glycosides was reported. Using cadmium carbonate as a catalyst in CH3CN, a series of saponins was synthesized efficiently in a satisfactory yield.
2003, 14(3): 233-234
Abstract:
The regioselective 1-O-deacylation of peracylated glycopyranoses 1a-d with zinc chloride and zinc oxide in THF/MeOH gave the corresponding tetra-O-acylglycopyranoses 2a-d in good yields.
The regioselective 1-O-deacylation of peracylated glycopyranoses 1a-d with zinc chloride and zinc oxide in THF/MeOH gave the corresponding tetra-O-acylglycopyranoses 2a-d in good yields.
2003, 14(3): 235-238
Abstract:
Unsymmetrical sulfides can be generated by the reaction of chlorine substituted aromatic compounds in sulfoxide in the presence of fluorine anion in fair yield. A likely mechanism was proposed.
Unsymmetrical sulfides can be generated by the reaction of chlorine substituted aromatic compounds in sulfoxide in the presence of fluorine anion in fair yield. A likely mechanism was proposed.
2003, 14(3): 239-242
Abstract:
Conducted in the ionic liquids, activated and inactivated halides, acyl chlorides, tosylate, and bezotriazolyl acylates were converted to corresponding azide and thiocyanide compounds in high yields under mild conditions.
Conducted in the ionic liquids, activated and inactivated halides, acyl chlorides, tosylate, and bezotriazolyl acylates were converted to corresponding azide and thiocyanide compounds in high yields under mild conditions.
2003, 14(3): 243-244
Abstract:
Phosphonium or arsonium salt 1 can undergo the tandem reaction of deprotonation-oxidation-Wittig reaction with alcohol 2 in the presence of sodium hydroxide and manganese dioxide, which affords a general simplified method for the stereoselective synthesis of (E)-α,β-unsaturated esters 3.
Phosphonium or arsonium salt 1 can undergo the tandem reaction of deprotonation-oxidation-Wittig reaction with alcohol 2 in the presence of sodium hydroxide and manganese dioxide, which affords a general simplified method for the stereoselective synthesis of (E)-α,β-unsaturated esters 3.
2003, 14(3): 245-246
Abstract:
The reverse atom transfer radical polymerization(RATRP) of (-)-menthyl methacrylate ((-)-MnMA) with AIBN(AIBN/CuCl2/bipyridine(bipy) or (-)sparteine((-)Sp)=1/2/4) initiating system in THF has been studied. The dependence of the specific rotation on molecular weight was investigated.
The reverse atom transfer radical polymerization(RATRP) of (-)-menthyl methacrylate ((-)-MnMA) with AIBN(AIBN/CuCl2/bipyridine(bipy) or (-)sparteine((-)Sp)=1/2/4) initiating system in THF has been studied. The dependence of the specific rotation on molecular weight was investigated.
2003, 14(3): 247-248
Abstract:
The solid phase synthesis of 4H-pyrimido[2,1-b] benzothiazol-4-ones has been reported.
The solid phase synthesis of 4H-pyrimido[2,1-b] benzothiazol-4-ones has been reported.
2003, 14(3): 249-250
Abstract:
Facile synthesis of 16-hydroxygeranylgeranio 1, a naturally occurring alicyclic diterpene, by alkylation reaction of allylic iodide 3 with phenyl sulfone 4, is described.
Facile synthesis of 16-hydroxygeranylgeranio 1, a naturally occurring alicyclic diterpene, by alkylation reaction of allylic iodide 3 with phenyl sulfone 4, is described.
2003, 14(3): 251-254
Abstract:
The two diarylheptanoids (E)-1-(4'-hydroxy-3'-methoxyphenyl)-7-(4"-hydroxyphenyl) hept-4-en-3-one 1 (Gingerenone C) and (±)-5-hydroxy-1-(4'-hydroxy-3'-methoxyphenyl)-7-(4"-hydroxyphenyl)-3-heptanone 2 were synthesized from vanillin 3 and 4-hydroxybenzaldehyde 9.
The two diarylheptanoids (E)-1-(4'-hydroxy-3'-methoxyphenyl)-7-(4"-hydroxyphenyl) hept-4-en-3-one 1 (Gingerenone C) and (±)-5-hydroxy-1-(4'-hydroxy-3'-methoxyphenyl)-7-(4"-hydroxyphenyl)-3-heptanone 2 were synthesized from vanillin 3 and 4-hydroxybenzaldehyde 9.
2003, 14(3): 255-256
Abstract:
Hydrozirconation of propargyl selenides afford (E)-3-selanyl vinylzirconocenes chlorides 2. Intermediates 2 reacted with aldehydes to obtain δ-selanyl allylic alcohols.
Hydrozirconation of propargyl selenides afford (E)-3-selanyl vinylzirconocenes chlorides 2. Intermediates 2 reacted with aldehydes to obtain δ-selanyl allylic alcohols.
2003, 14(3): 257-258
Abstract:
Two novel iron-based catalysts have been synthesized with high catalytic activity (about 108g oligomers/molFe·h) for ethylene oligomerization.
Two novel iron-based catalysts have been synthesized with high catalytic activity (about 108g oligomers/molFe·h) for ethylene oligomerization.
2003, 14(3): 259-262
Abstract:
The site of attachment of protein carrier to corticosteroids has great influence on the specificity of produced antibody. In order to obtain highly specific and accurate antibodies for bioimmunoassay determination of cortisol, different tether lengths of 6α-corticosteroid haptens and their BSA conjugates were designed and synthesized.
The site of attachment of protein carrier to corticosteroids has great influence on the specificity of produced antibody. In order to obtain highly specific and accurate antibodies for bioimmunoassay determination of cortisol, different tether lengths of 6α-corticosteroid haptens and their BSA conjugates were designed and synthesized.
2003, 14(3): 263-266
Abstract:
Two new blue luminescent zinc and beryllium complexes with Schiff base calixarene derivative as the ligand were prepared. Their luminescent properties were determined, which indicated that they had strong blue fluorescent properties. They also had good solubility and film formation. These new complexes can be used as blue organic electroluminescent materials (OELMs) in organic electroluminescent devices.
Two new blue luminescent zinc and beryllium complexes with Schiff base calixarene derivative as the ligand were prepared. Their luminescent properties were determined, which indicated that they had strong blue fluorescent properties. They also had good solubility and film formation. These new complexes can be used as blue organic electroluminescent materials (OELMs) in organic electroluminescent devices.
2003, 14(3): 267-269
Abstract:
Macroporous poly (vinyl acetate-co-triallyl isocyanurate) beads were prepared with suspension polymerization method. The copolymer beads were then transformed into poly (vinyl alcohol-co-triallyl isocyanurate) by ester exchange reaction. Aminocarboxylic acids were immobilized on the copolymer beads by the esterification of hydroxyl groups with diethyl-lenetriaminepentaacetic bisanhydride. The weak acid exchange capacities, specific surface areas and mean pore diameters of the resultant resin beads were measured.
Macroporous poly (vinyl acetate-co-triallyl isocyanurate) beads were prepared with suspension polymerization method. The copolymer beads were then transformed into poly (vinyl alcohol-co-triallyl isocyanurate) by ester exchange reaction. Aminocarboxylic acids were immobilized on the copolymer beads by the esterification of hydroxyl groups with diethyl-lenetriaminepentaacetic bisanhydride. The weak acid exchange capacities, specific surface areas and mean pore diameters of the resultant resin beads were measured.
2003, 14(3): 270-273
Abstract:
CIDNP techniques were applied to study the mechanism of photocycloadditions of 2-chloro-5-methoxybenzoquinone 1 with arylacetylenes 2-5 in benzene-d6 and acetonitrile-d6 respectively.
CIDNP techniques were applied to study the mechanism of photocycloadditions of 2-chloro-5-methoxybenzoquinone 1 with arylacetylenes 2-5 in benzene-d6 and acetonitrile-d6 respectively.
2003, 14(3): 274-275
Abstract:
A new dihydrochromone derivative, named chaenomone, was isolated from the twigs of Chaenomeles sinensis (Thouin) Koehne. The structure was determined by spectroscopic methods.
A new dihydrochromone derivative, named chaenomone, was isolated from the twigs of Chaenomeles sinensis (Thouin) Koehne. The structure was determined by spectroscopic methods.
2003, 14(3): 276-277
Abstract:
A new bibenzyl glycoside has been isolated from the stems of Dendrobium moniliforme (L.) Sw. (Orchidaceae). Its structure has been identified on the basis of spectroscopic and chemical methods.
A new bibenzyl glycoside has been isolated from the stems of Dendrobium moniliforme (L.) Sw. (Orchidaceae). Its structure has been identified on the basis of spectroscopic and chemical methods.
2003, 14(3): 278-279
Abstract:
A new dendrobine-type alkaloid has been isolated from stems of Dendrobium nobile lindl.. Its structure has been identified on the basis of spectroscopic method.
A new dendrobine-type alkaloid has been isolated from stems of Dendrobium nobile lindl.. Its structure has been identified on the basis of spectroscopic method.
2003, 14(3): 280-282
Abstract:
Erythromycin as a new chiral selector was first used for chrial separation of four derivatives of biphenyldimethylester enantiomers on CE. The influence of pH, the chiral selector concentration and organic modifiers were preliminarily studied. Experiments show that the erythromycin as chiral selector is useful to CE.
Erythromycin as a new chiral selector was first used for chrial separation of four derivatives of biphenyldimethylester enantiomers on CE. The influence of pH, the chiral selector concentration and organic modifiers were preliminarily studied. Experiments show that the erythromycin as chiral selector is useful to CE.
2003, 14(3): 283-286
Abstract:
A new chemiluminescence flow system has been developed for sequential determina-tion of benzoic acid based on the reaction of the compound with copper carbonate entrapped in a solid-phase reactor. It was found that the unsaturated complex of Cu(Ⅱ) and benzoic acid (1:1) has strong catalytic effect on the luminol-H2O2 chemiluminescence reaction. The calibration graph is linear over the range of 0.025~60 μg/mL of benzoic acid, with a relative standard deviation of less than 3.0%, and the detection limit is 0.01μg·mL-1. The proposed method was applied to the determination of benzoic acid content in different pharmaceutical formulations.
A new chemiluminescence flow system has been developed for sequential determina-tion of benzoic acid based on the reaction of the compound with copper carbonate entrapped in a solid-phase reactor. It was found that the unsaturated complex of Cu(Ⅱ) and benzoic acid (1:1) has strong catalytic effect on the luminol-H2O2 chemiluminescence reaction. The calibration graph is linear over the range of 0.025~60 μg/mL of benzoic acid, with a relative standard deviation of less than 3.0%, and the detection limit is 0.01μg·mL-1. The proposed method was applied to the determination of benzoic acid content in different pharmaceutical formulations.
2003, 14(3): 287-289
Abstract:
A sensitive method for the simultaneous determination of Cr(Ⅲ) and Cr(VI) using in-capillary reaction capillary electrophoresis separation and chemiluminescence detection was developed. The procedures were designed as follows:The sample, hydrochloric acid and sodium hydrogen sulfite solution segments were injected sequentially into the capillary. The reaction of Cr(VI) reduced to Cr(Ⅲ) by HSO3- occurred inside the capillary after applying the running voltage. According to the migration time difference of both Cr(Ⅲ) ions moving towards to the cathode (detection end), they could be separated and determined. The limits of detection for chromium(Ⅲ) and chromium(VI) (S/N=3) were 6.0×10-13 mol/L (12 zmol) and 1.9×10-11 mol/L (380 zmol), respectively.
A sensitive method for the simultaneous determination of Cr(Ⅲ) and Cr(VI) using in-capillary reaction capillary electrophoresis separation and chemiluminescence detection was developed. The procedures were designed as follows:The sample, hydrochloric acid and sodium hydrogen sulfite solution segments were injected sequentially into the capillary. The reaction of Cr(VI) reduced to Cr(Ⅲ) by HSO3- occurred inside the capillary after applying the running voltage. According to the migration time difference of both Cr(Ⅲ) ions moving towards to the cathode (detection end), they could be separated and determined. The limits of detection for chromium(Ⅲ) and chromium(VI) (S/N=3) were 6.0×10-13 mol/L (12 zmol) and 1.9×10-11 mol/L (380 zmol), respectively.
2003, 14(3): 290-293
Abstract:
A new method for indirect determination of cetyl-trimethyl ammonium bromide (CTMAB) with NaCl and NH4SCN by floatation and separation of zinc has been studied. The study shows that Zn(Ⅱ) can associate with NH4SCN and CTMAB to form insoluble ternary ion-association complex, and the precipitate can float on the surface of the liquid phase. A good linear relationship is observed between the floatation yield (E%) of Zn(Ⅱ) and the amount of CTMAB. On the ground, CTMAB can be indirectly determined by determining E% of Zn(Ⅱ). The results were satisfactory.
A new method for indirect determination of cetyl-trimethyl ammonium bromide (CTMAB) with NaCl and NH4SCN by floatation and separation of zinc has been studied. The study shows that Zn(Ⅱ) can associate with NH4SCN and CTMAB to form insoluble ternary ion-association complex, and the precipitate can float on the surface of the liquid phase. A good linear relationship is observed between the floatation yield (E%) of Zn(Ⅱ) and the amount of CTMAB. On the ground, CTMAB can be indirectly determined by determining E% of Zn(Ⅱ). The results were satisfactory.
2003, 14(3): 294-297
Abstract:
The contributions of tetrahydrofurfuryl alcohol (THFA) and polyethylene glycol (PEG) to the renatured efficiency of α-chymotrypsin were investigated and compared with each other. The maximum increments of bioactivity recovery of α-Chy were found to be 25.1% for THFA, 10.4% for PEG, respectively. The experimental results indicated that the denaturant solution containing THFA contributed more to the renaturation of α-Chy in high performance hydrophobic interaction chromatography (HPHIC) than that containing PEG, when the concentration of THFA was 3.2%, the bioactivity recovery of α-Chy is the highest.
The contributions of tetrahydrofurfuryl alcohol (THFA) and polyethylene glycol (PEG) to the renatured efficiency of α-chymotrypsin were investigated and compared with each other. The maximum increments of bioactivity recovery of α-Chy were found to be 25.1% for THFA, 10.4% for PEG, respectively. The experimental results indicated that the denaturant solution containing THFA contributed more to the renaturation of α-Chy in high performance hydrophobic interaction chromatography (HPHIC) than that containing PEG, when the concentration of THFA was 3.2%, the bioactivity recovery of α-Chy is the highest.
2003, 14(3): 298-299
Abstract:
The configurations of substituted phenyl furoisoxazolines were determined by study on their 1H-NMR and 1D NOESY. The characteristic chemical shifts of the γ-lactone ring protons in 1H-NMR were also discussed.
The configurations of substituted phenyl furoisoxazolines were determined by study on their 1H-NMR and 1D NOESY. The characteristic chemical shifts of the γ-lactone ring protons in 1H-NMR were also discussed.
2003, 14(3): 300-303
Abstract:
A new method for the study of triplex DNA is established according the fluorescence enhancement of molecular "Light Switch" complex of Ru(phen)2(dppx)2+ when it intercalate into triplex DNA. Because the fluorescence intensity of Ru(phen)2(dppx)2+ bonded to triplex DNA is in the case higher than that bonded to duplex DNA in certain range of DNA concentration, the method is much more sensitive than other methods reported previously.
A new method for the study of triplex DNA is established according the fluorescence enhancement of molecular "Light Switch" complex of Ru(phen)2(dppx)2+ when it intercalate into triplex DNA. Because the fluorescence intensity of Ru(phen)2(dppx)2+ bonded to triplex DNA is in the case higher than that bonded to duplex DNA in certain range of DNA concentration, the method is much more sensitive than other methods reported previously.
2003, 14(3): 304-307
Abstract:
Capillary zone electrophoresis (CZE) was applied to study the interaction between netropsin and a 14mer double stranded DNA (dsDNA). The binding constant of this interaction calculated from Scatchard plot was (1.07±0.10)×105 (mol/L)-1. The binding stoichiometry was 1:1. The use of polyacrylamide coated capillary showed better effect in the analysis of DNA than noncoated capillary.
Capillary zone electrophoresis (CZE) was applied to study the interaction between netropsin and a 14mer double stranded DNA (dsDNA). The binding constant of this interaction calculated from Scatchard plot was (1.07±0.10)×105 (mol/L)-1. The binding stoichiometry was 1:1. The use of polyacrylamide coated capillary showed better effect in the analysis of DNA than noncoated capillary.
2003, 14(3): 308-311
Abstract:
A new method for preparing effective inhibition film on copper has been developed. Phenylthiourea (PT) was first absorbed to copper surface to form a monolayer. 1-Dodecanethiol (DT) was then assembled on the surface for modification. Finally, AC voltage was loaded on copper covered the mixed film to improve it further. After these processes, an effective inhibition film was gained because of its high charge transfer resistance and low corrosion current density shown in electrochemical impedance spectra and polarization. The inhibition efficiency was more than 97%.
A new method for preparing effective inhibition film on copper has been developed. Phenylthiourea (PT) was first absorbed to copper surface to form a monolayer. 1-Dodecanethiol (DT) was then assembled on the surface for modification. Finally, AC voltage was loaded on copper covered the mixed film to improve it further. After these processes, an effective inhibition film was gained because of its high charge transfer resistance and low corrosion current density shown in electrochemical impedance spectra and polarization. The inhibition efficiency was more than 97%.
2003, 14(3): 312-315
Abstract:
Non-carbon inorganic fullerene-like (IF) nanoscale materials have recently attracted intense interest due to their nested hollow and nanotube structures. In this letter, IF-WS2 nanoparticles prepared by solid-gas reaction were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results show that the IF-WS2 nanoparticles have a nested hollow closed spherical structure with diameter of 100-150 nm.
Non-carbon inorganic fullerene-like (IF) nanoscale materials have recently attracted intense interest due to their nested hollow and nanotube structures. In this letter, IF-WS2 nanoparticles prepared by solid-gas reaction were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results show that the IF-WS2 nanoparticles have a nested hollow closed spherical structure with diameter of 100-150 nm.
2003, 14(3): 316-318
Abstract:
The characteristic parameters were measured with floating double probe method when cold plasma was interacting with catalysts, such as MoO3/Al2O3, NiY, Pd/Al2O3, which were used in the conversion of natural gas to C2 hydrocarbons through electrical field enhanced plasma catalysis. These parameters were compared in different input voltage, different atmosphere, before and after reaction in plasma field. The interaction between catalysts and cold plasma was also investigated. This confirm that cold plasma can enhanced catalysis effect.
The characteristic parameters were measured with floating double probe method when cold plasma was interacting with catalysts, such as MoO3/Al2O3, NiY, Pd/Al2O3, which were used in the conversion of natural gas to C2 hydrocarbons through electrical field enhanced plasma catalysis. These parameters were compared in different input voltage, different atmosphere, before and after reaction in plasma field. The interaction between catalysts and cold plasma was also investigated. This confirm that cold plasma can enhanced catalysis effect.
2003, 14(3): 319-322
Abstract:
The Pd-B/γ-Al2O3 amorphous alloy catalyst and Pd/γ-Al2O3 crystalline metal catalyst were prepared by KBH4 reduction and routine impregnation, respectively. Pd-B/γ-A12O3 and Pd/γ-A12O3 catalysts were characterized by XRD and SEM. It was found that the catalytic activity of the Pd-B/γ-A12O3 amorphous alloy catalyst was higher than that of the Pd/γ-A12O3crystalline metal catalyst in the anthraquinone hydrogenation.
The Pd-B/γ-Al2O3 amorphous alloy catalyst and Pd/γ-Al2O3 crystalline metal catalyst were prepared by KBH4 reduction and routine impregnation, respectively. Pd-B/γ-A12O3 and Pd/γ-A12O3 catalysts were characterized by XRD and SEM. It was found that the catalytic activity of the Pd-B/γ-A12O3 amorphous alloy catalyst was higher than that of the Pd/γ-A12O3crystalline metal catalyst in the anthraquinone hydrogenation.
2003, 14(3): 323-326
Abstract:
Monodisperse a-Fe2O3 particles with different particle size (ca. 620±10 nm or 60±4 nm) have been successfully prepared by hydrothermal method in short periods. In this process, the crystal-growing inhibitor (DBS) favored the formation of monodisperse nanoparticles.
Monodisperse a-Fe2O3 particles with different particle size (ca. 620±10 nm or 60±4 nm) have been successfully prepared by hydrothermal method in short periods. In this process, the crystal-growing inhibitor (DBS) favored the formation of monodisperse nanoparticles.
2003, 14(3): 327-330
Abstract:
Spontaneous vesicles from the mixed aqueous solution of poly-tailed cationic surfactant PTA and anionic surfactant AOT are firstly obtained. Vesicle formation and characterizations are demonstrated by negative-staining TEM and dynamic light scattering. A monodisperse vesicle system is obtained with a polydispersity of 0.082. Ultrasonication can promote the vesicle formation. Mechanism of vesicle formation is discussed from the viewpoint of molecular interaction.
Spontaneous vesicles from the mixed aqueous solution of poly-tailed cationic surfactant PTA and anionic surfactant AOT are firstly obtained. Vesicle formation and characterizations are demonstrated by negative-staining TEM and dynamic light scattering. A monodisperse vesicle system is obtained with a polydispersity of 0.082. Ultrasonication can promote the vesicle formation. Mechanism of vesicle formation is discussed from the viewpoint of molecular interaction.
