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1999 Volume 10 Issue 2
1999, 10(2): 95-96
Abstract:
C60,derivatives covalently linked with the nitroxide radical of 2, 2, 6, 6-tetramethylpiperidine-1-oxyl have been synthesized by the following new method: C60 reacts with 4-oxo-2, 2, 6, 6-tetramethyl-piperidinyloxyl (4-oxo-TEMPO) and an amino acid.
C60,derivatives covalently linked with the nitroxide radical of 2, 2, 6, 6-tetramethylpiperidine-1-oxyl have been synthesized by the following new method: C60 reacts with 4-oxo-2, 2, 6, 6-tetramethyl-piperidinyloxyl (4-oxo-TEMPO) and an amino acid.
1999, 10(2): 97-98
Abstract:
A new and simple procedure for the synthesis of aliphatic α-organothio aldoximes was reported. The aliphatic aldoxime was chlorinated by t-BuOCl, the resulting hydroxime acid chloride was treated with triethylamine and alkyl mercaptan in a one pot procedure to get the target compounds. The method is very efficient with high yield and good purity.
A new and simple procedure for the synthesis of aliphatic α-organothio aldoximes was reported. The aliphatic aldoxime was chlorinated by t-BuOCl, the resulting hydroxime acid chloride was treated with triethylamine and alkyl mercaptan in a one pot procedure to get the target compounds. The method is very efficient with high yield and good purity.
1999, 10(2): 99-100
Abstract:
A new boron complex of calix[4Jarene was synthesized by the reaction of calix [4] arene with BMS; and the structure of the product was characterized by IR,1HNMR, 13CNMR, 11BNMR and MS spectra.
A new boron complex of calix[4Jarene was synthesized by the reaction of calix [4] arene with BMS; and the structure of the product was characterized by IR,1HNMR, 13CNMR, 11BNMR and MS spectra.
1999, 10(2): 101-102
Abstract:
Traps-2,2-dimethyl-3一(2,2-dichloroethenyl) cyclopropanecarbonyl chloride, which is an important intermediate for insecticides, is obtained by isomerization of the cis/traps-mixture with 4- (N,N-dimethylamino) pyridine (DMAP) in the presence or absence of halogen compounds in good yield.
Traps-2,2-dimethyl-3一(2,2-dichloroethenyl) cyclopropanecarbonyl chloride, which is an important intermediate for insecticides, is obtained by isomerization of the cis/traps-mixture with 4- (N,N-dimethylamino) pyridine (DMAP) in the presence or absence of halogen compounds in good yield.
1999, 10(2): 103-104
Abstract:
5-Phenyl-4-aroylfuran-3-carboxylic acids were reduced in aqueous alkaline solutions of NaBH4 to afford hydroxy acids in excellent yields. Under the catalysis of boron trifluoride etherate, the hydroxy acids were converted to lactones smoothly.
5-Phenyl-4-aroylfuran-3-carboxylic acids were reduced in aqueous alkaline solutions of NaBH4 to afford hydroxy acids in excellent yields. Under the catalysis of boron trifluoride etherate, the hydroxy acids were converted to lactones smoothly.
1999, 10(2): 105-106
Abstract:
(4S)-4-Carboxyl-I-oxoperoxovanatrane and (4S)-3-methyl-4-carboxyl-l-oxoperoxovanatrane were synthesized from the reaction of potassium vanadate, hydrogen peroxide with L-N, N-bis (2-hydroxyethyl) serine or L-N. N-bis (2-hydroxyethyl) threonine in water.
(4S)-4-Carboxyl-I-oxoperoxovanatrane and (4S)-3-methyl-4-carboxyl-l-oxoperoxovanatrane were synthesized from the reaction of potassium vanadate, hydrogen peroxide with L-N, N-bis (2-hydroxyethyl) serine or L-N. N-bis (2-hydroxyethyl) threonine in water.
1999, 10(2): 107-108
Abstract:
2-(4-Hydroxyphenyl)-3-hydroxymethyl-l,4-benzodioxane-6-aldehyde 8, the key intermediate of sinaiticin 10. was synthesized in 6 steps from caffeic acid 4 and 4-hydroxybenzaldehyde 1, the coupling reaction is the key step.
2-(4-Hydroxyphenyl)-3-hydroxymethyl-l,4-benzodioxane-6-aldehyde 8, the key intermediate of sinaiticin 10. was synthesized in 6 steps from caffeic acid 4 and 4-hydroxybenzaldehyde 1, the coupling reaction is the key step.
1999, 10(2): 109-110
Abstract:
3一(3-hydroxypropyl)-phthalide 1, a phthalide isolated from the flowers of G. pedicellata Wall, has been synthesized in high yield from 2-carboxybenzaldehyde 3 in 2 steps. Reaction of 1 with 2,3-dihydroxybenzoic acid afforded pedicellosine 2, another phthalide from the leaves of G pedicellata Wall.
3一(3-hydroxypropyl)-phthalide 1, a phthalide isolated from the flowers of G. pedicellata Wall, has been synthesized in high yield from 2-carboxybenzaldehyde 3 in 2 steps. Reaction of 1 with 2,3-dihydroxybenzoic acid afforded pedicellosine 2, another phthalide from the leaves of G pedicellata Wall.
1999, 10(2): 111-112
Abstract:
A total synthesis of (3S, 6S)- (+)-3,7-dimethyl-3-acetoxy-6-hydroxy-octa-l,7-diene via the rearrangement of chiral 2,3-epoxy alcohol, with the system of Ph3P, pyridine, I2 and H20, is described.
A total synthesis of (3S, 6S)- (+)-3,7-dimethyl-3-acetoxy-6-hydroxy-octa-l,7-diene via the rearrangement of chiral 2,3-epoxy alcohol, with the system of Ph3P, pyridine, I2 and H20, is described.
1999, 10(2): 113-114
Abstract:
A series of 1,2-cyclic monoacyl-rac-glycerothiophosphates of cantharidin and its analogues were synthesized in a one-pot procedure in overall yields of 44~55.5% by means of hexaethylphosphorus triamide as phosphorylating reagent.
A series of 1,2-cyclic monoacyl-rac-glycerothiophosphates of cantharidin and its analogues were synthesized in a one-pot procedure in overall yields of 44~55.5% by means of hexaethylphosphorus triamide as phosphorylating reagent.
Synthesis, Structure and Antitumor Activities of Tridccapeptide PSPP3 from Papaver Somniferum Pollen
1999, 10(2): 115-116
Abstract:
Five analogs and five segments of the Papavor Somniferum pollen tridecapeptide PSPP3 were designed and synthesised by using solid-phase peptide synthesis method. Their inhibitive activities to human liver tumor cell Bel-7402 were assayed by MTT method and their secondary structures in solution were determined by CD spectra. The relationship of the structure and activity was discussed.
Five analogs and five segments of the Papavor Somniferum pollen tridecapeptide PSPP3 were designed and synthesised by using solid-phase peptide synthesis method. Their inhibitive activities to human liver tumor cell Bel-7402 were assayed by MTT method and their secondary structures in solution were determined by CD spectra. The relationship of the structure and activity was discussed.
1999, 10(2): 117-120
Abstract:
1,2-O-Isopropylidene-3-C-cyano-5-O-benzoyl-α-D-xylose 2 was prepared stereoselectively from 1,2-O-isopropylidene-3-oxo-5-O-benzoyl-α-D-xylose 1. The structure of 2 was studied by two-dimensional NMR spectroscopy in conjunction with X-ray crystallography of its corresponding 5-phenyl-1.2,4-oxadiazole isocarbonucleoside derivative 3. The absolute configurations of 2 and 3, and conformation of 3 are described herein.
1,2-O-Isopropylidene-3-C-cyano-5-O-benzoyl-α-D-xylose 2 was prepared stereoselectively from 1,2-O-isopropylidene-3-oxo-5-O-benzoyl-α-D-xylose 1. The structure of 2 was studied by two-dimensional NMR spectroscopy in conjunction with X-ray crystallography of its corresponding 5-phenyl-1.2,4-oxadiazole isocarbonucleoside derivative 3. The absolute configurations of 2 and 3, and conformation of 3 are described herein.
1999, 10(2): 121-122
Abstract:
The monoclonal antibody ID11D7 to carboxypeptidase A (CPA) was prepared. The inhibitory effect of McAb ID11D7 on the peptidase activity of CPA was measured. The result reflects that the McAb ID11D7 can competitively inhibit the peptidase activity of CPA with an apparent inhibitory constant of 6.3 × 10-9M. Based on this work, the McAb ID11D7 can be used as idiotypic antigen to prepare anti-idiotypic catalytic antibody with the peptidase activity similar to CPA.
The monoclonal antibody ID11D7 to carboxypeptidase A (CPA) was prepared. The inhibitory effect of McAb ID11D7 on the peptidase activity of CPA was measured. The result reflects that the McAb ID11D7 can competitively inhibit the peptidase activity of CPA with an apparent inhibitory constant of 6.3 × 10-9M. Based on this work, the McAb ID11D7 can be used as idiotypic antigen to prepare anti-idiotypic catalytic antibody with the peptidase activity similar to CPA.
1999, 10(2): 123-124
Abstract:
Electrochemistry of didodecyldimethylannnonium bromide (DDAR) films containing cobalt phthalocyanine tetrasulfonate (CoPcTS4-) was examined. CoPcTS4--DDAB film electrode showed stable cyclic voltanunetric responses in butlers and could catalyze reductions of trichloroacetic acid.
Electrochemistry of didodecyldimethylannnonium bromide (DDAR) films containing cobalt phthalocyanine tetrasulfonate (CoPcTS4-) was examined. CoPcTS4--DDAB film electrode showed stable cyclic voltanunetric responses in butlers and could catalyze reductions of trichloroacetic acid.
1999, 10(2): 125-126
Abstract:
Erigeside 1 was isolated trom Erigeron breviscapus. The structure elucidation and 1H13C NMR assignments were achieved by spectroscopic method.
Erigeside 1 was isolated trom Erigeron breviscapus. The structure elucidation and 1H13C NMR assignments were achieved by spectroscopic method.
1999, 10(2): 127-128
Abstract:
An efficient NMR determination of the enantiomeric excess of the amino acids can be achieved using chloro-bridged dimer R- (+) -{Pd [η5-C5H5)Fe (η5-C5H3CMe=NAr)] (μ-Cl)}2(Ar=p-CH3C6H4) (R-1).
An efficient NMR determination of the enantiomeric excess of the amino acids can be achieved using chloro-bridged dimer R- (+) -{Pd [η5-C5H5)Fe (η5-C5H3CMe=NAr)] (μ-Cl)}2(Ar=p-CH3C6H4) (R-1).
1999, 10(2): 129-130
Abstract:
A new nor-neolignan, named ellisinin A (1), has been isolated from the traditional Tibetan medicinal plants of Cremanthodium ellisii. Its structure has been determined on the basis of spectroscopic evidence, especially by 2DNMR (1H-1HCOSY, HMQC, HMBC)
A new nor-neolignan, named ellisinin A (1), has been isolated from the traditional Tibetan medicinal plants of Cremanthodium ellisii. Its structure has been determined on the basis of spectroscopic evidence, especially by 2DNMR (1H-1HCOSY, HMQC, HMBC)
1999, 10(2): 131-132
Abstract:
A new dopamine derivative, lyciumide A, was isolated from the fruits of Lycium bnrbarum. Its structure was elucidated as p-methoxy-cis-cinnamoyl dopamine by spectral methods
A new dopamine derivative, lyciumide A, was isolated from the fruits of Lycium bnrbarum. Its structure was elucidated as p-methoxy-cis-cinnamoyl dopamine by spectral methods
1999, 10(2): 133-134
Abstract:
Two new diterpenoid alkaloids have been isolated from roots of Aconitum excelsum Reichb. These new compounds were named excecoitine I and exceconidine II. The two structures were elucidated by spectroscopic methods as well as comparison with known compounds.
Two new diterpenoid alkaloids have been isolated from roots of Aconitum excelsum Reichb. These new compounds were named excecoitine I and exceconidine II. The two structures were elucidated by spectroscopic methods as well as comparison with known compounds.
1999, 10(2): 135-138
Abstract:
Three new styrylpyrones, named 7-epi-goniodiol 1, leiocarpin B 2 and leiocarpin C 3. were isolated trom the stem barks of Goniothalamus leiocarpus. Their structures were elucidated by means of spectral and chemical methods. The relative configuration of 1 and 2 were determined by X-ray crystallographic analysis.
Three new styrylpyrones, named 7-epi-goniodiol 1, leiocarpin B 2 and leiocarpin C 3. were isolated trom the stem barks of Goniothalamus leiocarpus. Their structures were elucidated by means of spectral and chemical methods. The relative configuration of 1 and 2 were determined by X-ray crystallographic analysis.
1999, 10(2): 139-142
Abstract:
Erythrinarbine 2, a novel alkaloid was isolated from the stem of Erythrina arborescens Roxb. Its structure and stereochemistry were elucidated on the basis of the spectral analysis (13C-1H COSY. 1H-1H COSY, NOESY and HMBC).
Erythrinarbine 2, a novel alkaloid was isolated from the stem of Erythrina arborescens Roxb. Its structure and stereochemistry were elucidated on the basis of the spectral analysis (13C-1H COSY. 1H-1H COSY, NOESY and HMBC).
1999, 10(2): 143-144
Abstract:
Trimethylchlorosilane was used as a stereoselective reagent to determine the a or a orientation of 3-hydroxyl group of some steroids by chemical ionization mass spectrometry.
Trimethylchlorosilane was used as a stereoselective reagent to determine the a or a orientation of 3-hydroxyl group of some steroids by chemical ionization mass spectrometry.
1999, 10(2): 145-146
Abstract:
The intermolecular interaction in an azobenzene self-assembled monolayers (SAMs) on gold electrode was investigated by controlling the assembling time and using mixed self-assembled techniques, and the variation of apparent electron transfer rate constant (ks) of azobenzene SAMs with different molecular packing density is reported.
The intermolecular interaction in an azobenzene self-assembled monolayers (SAMs) on gold electrode was investigated by controlling the assembling time and using mixed self-assembled techniques, and the variation of apparent electron transfer rate constant (ks) of azobenzene SAMs with different molecular packing density is reported.
1999, 10(2): 147-150
Abstract:
In this paper, it is the first time to report the study on the state-to-state rotational energy transfer (RET)of NH2 (Ã2 A1;0,9,0) under molecular beam condition in detail. Through a systematic study of the relative population transferred as functions of initially excited quantum state, including different Ka, nuclear-spin, and even spin-doublet, some propensity rules were obtained directly.
In this paper, it is the first time to report the study on the state-to-state rotational energy transfer (RET)of NH2 (Ã2 A1;0,9,0) under molecular beam condition in detail. Through a systematic study of the relative population transferred as functions of initially excited quantum state, including different Ka, nuclear-spin, and even spin-doublet, some propensity rules were obtained directly.
1999, 10(2): 151-154
Abstract:
A highly efficient copolymer (methacrylic acid-co-styrene-divinylbenzene) in situ making high-performance liquid chromatographic column was prepared and evaluated. The column efficiency calculated in terms of height equivalent to a theoretical plate was 25 pm and rapid separations of small molecules such as substituted aromatic hydrocarbons and aromatic acids were achieved within five minutes.
A highly efficient copolymer (methacrylic acid-co-styrene-divinylbenzene) in situ making high-performance liquid chromatographic column was prepared and evaluated. The column efficiency calculated in terms of height equivalent to a theoretical plate was 25 pm and rapid separations of small molecules such as substituted aromatic hydrocarbons and aromatic acids were achieved within five minutes.
1999, 10(2): 155-156
Abstract:
It was shown that a new sensitive spectrophotometric method for the determination of trace arsenic with chlorpromazine by the formation of heteropoly arsenomolybdic chlorpromazine complex in aqueous phase.
It was shown that a new sensitive spectrophotometric method for the determination of trace arsenic with chlorpromazine by the formation of heteropoly arsenomolybdic chlorpromazine complex in aqueous phase.
1999, 10(2): 157-160
Abstract:
CT-DNA were electrochemically immobilized on the surfaces of both nano-gold modified glassy carbon electrode and bare glassy carbon electrode. The cyclic voltammetrie behavior of Co (phen)33+ adsorbed on the immobilized DNA was studied. Increase in the peak current of Co (phen)33+ redox reaction was obtained on nano-gold modified glassy carbon electrode. The result suggests that more DNA molecules were immobilized on this electrode and nano-gold modification can enhance the heterogeneous electron transfer rate constant of the Co (phen)33+.
CT-DNA were electrochemically immobilized on the surfaces of both nano-gold modified glassy carbon electrode and bare glassy carbon electrode. The cyclic voltammetrie behavior of Co (phen)33+ adsorbed on the immobilized DNA was studied. Increase in the peak current of Co (phen)33+ redox reaction was obtained on nano-gold modified glassy carbon electrode. The result suggests that more DNA molecules were immobilized on this electrode and nano-gold modification can enhance the heterogeneous electron transfer rate constant of the Co (phen)33+.
1999, 10(2): 161-164
Abstract:
C60 is successfully solubilized in micelle of six kinds of surfactants and UV/Vis spectra of C60 in micellar system are studied. It is found that Brij-35 is the most efficient surfactant for solubilization of C60 and the possible states of C60 existed in surfactants are also studied. Experiments of surface tension show that the sites for solubilization of C60 not only depend on the sorts of surfactants but also on their structures.
C60 is successfully solubilized in micelle of six kinds of surfactants and UV/Vis spectra of C60 in micellar system are studied. It is found that Brij-35 is the most efficient surfactant for solubilization of C60 and the possible states of C60 existed in surfactants are also studied. Experiments of surface tension show that the sites for solubilization of C60 not only depend on the sorts of surfactants but also on their structures.
1999, 10(2): 165-166
Abstract:
It was found for the first time that gramicidin D (GD) molecules can be incorporated into the ODM monolayer which is self-assembled on the surface of the gold electrode and form monovalent canon channels.
It was found for the first time that gramicidin D (GD) molecules can be incorporated into the ODM monolayer which is self-assembled on the surface of the gold electrode and form monovalent canon channels.
1999, 10(2): 167-170
Abstract:
The potassium salt of monocarboxylic substituted .porphyrin and mono crown ether substituted phthalocyanine can form heterodimer in solution and this kind of heterodimer can be fabricated into highly ordered LB films. The structures of the film were identified by absorption spectra, polarized absorption spectra and low angle X-ray diffraction methods.
The potassium salt of monocarboxylic substituted .porphyrin and mono crown ether substituted phthalocyanine can form heterodimer in solution and this kind of heterodimer can be fabricated into highly ordered LB films. The structures of the film were identified by absorption spectra, polarized absorption spectra and low angle X-ray diffraction methods.
1999, 10(2): 171-174
Abstract:
Novel highly active n5-pentamethylcyclopentadienyltribenzyloxy titanium catalyst activated by modified methylaluminoxane (m-MAO) was prepared for styrene syndiospecific polymerization. The influences of the contents of trimethylaluminum (TMA) in m-MAO and external addition of tri-isobutylaluminum (TIBA) on the distribution of the oxidation states of titanium were investigated in detail. The Ti(III)is in favour of styrene syndiospecific polymerization in higher catalytic activity.
Novel highly active n5-pentamethylcyclopentadienyltribenzyloxy titanium catalyst activated by modified methylaluminoxane (m-MAO) was prepared for styrene syndiospecific polymerization. The influences of the contents of trimethylaluminum (TMA) in m-MAO and external addition of tri-isobutylaluminum (TIBA) on the distribution of the oxidation states of titanium were investigated in detail. The Ti(III)is in favour of styrene syndiospecific polymerization in higher catalytic activity.
1999, 10(2): 175-178
Abstract:
The kinetics of nonisothermal and isothermal crystallization of metallocene catalyzed and conventional polyethylenes has been studied by differential scanning calorimetry. Using Avrami equation, Ozawa theory and Mo Zhishen method, the experimental data have been analyzed. It is shown that metallocene polyethylene possesses a higher rate of crystallization due to a higher stereoregularity of its molecular chains. Moreover, they have different nonisothermal crystallization mechanisms and identical isothermal crystallization mechanisms.
The kinetics of nonisothermal and isothermal crystallization of metallocene catalyzed and conventional polyethylenes has been studied by differential scanning calorimetry. Using Avrami equation, Ozawa theory and Mo Zhishen method, the experimental data have been analyzed. It is shown that metallocene polyethylene possesses a higher rate of crystallization due to a higher stereoregularity of its molecular chains. Moreover, they have different nonisothermal crystallization mechanisms and identical isothermal crystallization mechanisms.
1999, 10(2): 179-182
Abstract:
Electrochemical oxidation of BEDT-TTF (bis (ethylenedithio) tetrathiafulvalene) in chloroform/carbon disulfide (3:1) in the presence of Bu4NBr as a supporting electrolyte at low current density results in the (BEDT-TTF)2Br3H20 crystal. Its composition has been established by chemical analysis (Br, C, H, S), XPS and IR. The temperature dependence of the resistance has been studied down to 26K at ambient pressure. This material has weakly metallic behavior above 230K, and becomes a semiconductor below this temperature. The structure of the complex is also described.
Electrochemical oxidation of BEDT-TTF (bis (ethylenedithio) tetrathiafulvalene) in chloroform/carbon disulfide (3:1) in the presence of Bu4NBr as a supporting electrolyte at low current density results in the (BEDT-TTF)2Br3H20 crystal. Its composition has been established by chemical analysis (Br, C, H, S), XPS and IR. The temperature dependence of the resistance has been studied down to 26K at ambient pressure. This material has weakly metallic behavior above 230K, and becomes a semiconductor below this temperature. The structure of the complex is also described.
1999, 10(2): 183-184
Abstract:
Five lanthanide porphyrin complexes with 5-(4-nitrophenyl)-10, 15, 20-triphenyl porphyrin and acetylacetonate ligands were synthesized and characterized by elemental analysis, IR spectra, Uv-visible spectra, 1H NMR. The structures of the complexes were proposed.
Five lanthanide porphyrin complexes with 5-(4-nitrophenyl)-10, 15, 20-triphenyl porphyrin and acetylacetonate ligands were synthesized and characterized by elemental analysis, IR spectra, Uv-visible spectra, 1H NMR. The structures of the complexes were proposed.
1999, 10(2): 185-186
Abstract:
The photochromism in CaS:Sm (from white to pink) was observed for the first time by exposing it to ultraviolet light. The experiments results show that the absorption intensity of Sm2+ in the range of 500~600nm was strongly increased after irradiation. valence changing of Sm. If the sample was excited by visible light This reveals that there is the again, the pink color turned to white, indicating that CaS:Sm has potential application in the field of storage material.
The photochromism in CaS:Sm (from white to pink) was observed for the first time by exposing it to ultraviolet light. The experiments results show that the absorption intensity of Sm2+ in the range of 500~600nm was strongly increased after irradiation. valence changing of Sm. If the sample was excited by visible light This reveals that there is the again, the pink color turned to white, indicating that CaS:Sm has potential application in the field of storage material.
1999, 10(2): 187-188
Abstract:
A novel mixed-valence copper (I, II) complex Cu3 [CH2=C(CH3) COO]5 (imH)3 (H2O) has been synthesized and characterised by XPS spectra and single crystal X-ray structural analysis The title complex crystallized in monoclinic space group P21/c, with a=11.225 (3), b=13.9023 (12) c=24.559 (2)Å, β=92.372 (10)° and Z=4. Final R=0.0495 for 5546 reflections [I>2σ(I)].
A novel mixed-valence copper (I, II) complex Cu3 [CH2=C(CH3) COO]5 (imH)3 (H2O) has been synthesized and characterised by XPS spectra and single crystal X-ray structural analysis The title complex crystallized in monoclinic space group P21/c, with a=11.225 (3), b=13.9023 (12) c=24.559 (2)Å, β=92.372 (10)° and Z=4. Final R=0.0495 for 5546 reflections [I>2σ(I)].
