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2002 Volume 13 Issue 2
2002, 13(2): 95-96
Abstract:
Acetophenone oxime and benzaldehyde oxime were converted to oxime ethers in the presence of alkyl halide or methyl sulfate and KOH in aqueous DMSO in 5 to 70 min.The yields of oxime ethers were 70-96%.
Acetophenone oxime and benzaldehyde oxime were converted to oxime ethers in the presence of alkyl halide or methyl sulfate and KOH in aqueous DMSO in 5 to 70 min.The yields of oxime ethers were 70-96%.
2002, 13(2): 97-100
Abstract:
The intermolecular coupling of a nitro group with a cyano group mediated by a Sm(Hg) amalgam prepared from metal samarium powder and catalytic mercury dichloride was studied.
The intermolecular coupling of a nitro group with a cyano group mediated by a Sm(Hg) amalgam prepared from metal samarium powder and catalytic mercury dichloride was studied.
2002, 13(2): 101-104
Abstract:
A very convenient construction procedure of the α, β-unsaturated lactone has been carried out in 98% yield.SmI2 (10%) was used as catalyst for rearrangement of an enol ester epoxide of eudesmanolide sesquiterpene.The possible mechanism was also discussed.
A very convenient construction procedure of the α, β-unsaturated lactone has been carried out in 98% yield.SmI2 (10%) was used as catalyst for rearrangement of an enol ester epoxide of eudesmanolide sesquiterpene.The possible mechanism was also discussed.
2002, 13(2): 105-106
Abstract:
α-Bromo benzoylmethylene triphenylphosphorane 3 has been synthesized by the reaction of benzoylmethylene triphenylphosphorane 1 with N-bromosuccinimide in the yield of 87% and can react with aromatic aldehydes 4 to give α-bromochalcones 5 in good yields.
α-Bromo benzoylmethylene triphenylphosphorane 3 has been synthesized by the reaction of benzoylmethylene triphenylphosphorane 1 with N-bromosuccinimide in the yield of 87% and can react with aromatic aldehydes 4 to give α-bromochalcones 5 in good yields.
2002, 13(2): 107-110
Abstract:
A novel Co-B amorphous alloy catalyst in the form of ultrafine particles was prepared by chemical reduction of CoCl2 with aqueous NaBH4, which exhibited excellent activity and selectivity during the hydrogenation of cinnamaldehyde to cinnamyl alcohol in liquid phase.The optimum yield of cinnamyl alcohol was 87.6%, much better than the yield of using Raney Ni, Raney Co and other Co-based catalysts.
A novel Co-B amorphous alloy catalyst in the form of ultrafine particles was prepared by chemical reduction of CoCl2 with aqueous NaBH4, which exhibited excellent activity and selectivity during the hydrogenation of cinnamaldehyde to cinnamyl alcohol in liquid phase.The optimum yield of cinnamyl alcohol was 87.6%, much better than the yield of using Raney Ni, Raney Co and other Co-based catalysts.
2002, 13(2): 111-112
Abstract:
The stereoselective synthesis of (2R, 4R)-2-N-tert-butyloxycarbonyl amino-4, 5-epoxido-valeric acid methyl ester 8, which is the key intermediate for the synthesis of (2'S, 2R)-3-trans-nitrocyclopropyl-alanine, was first accomplished.
The stereoselective synthesis of (2R, 4R)-2-N-tert-butyloxycarbonyl amino-4, 5-epoxido-valeric acid methyl ester 8, which is the key intermediate for the synthesis of (2'S, 2R)-3-trans-nitrocyclopropyl-alanine, was first accomplished.
2002, 13(2): 113-114
Abstract:
A new facile route for the synthesis of dl-shikonin is presented.Reformatsky reaction assisted cross-coupling of 1, 4, 5, 8-tetramethoxynaphthalene-2-carbaldehyde and ethyl-bromoacetate was employed for introduction of the side chain of dl-shikonin.
A new facile route for the synthesis of dl-shikonin is presented.Reformatsky reaction assisted cross-coupling of 1, 4, 5, 8-tetramethoxynaphthalene-2-carbaldehyde and ethyl-bromoacetate was employed for introduction of the side chain of dl-shikonin.
2002, 13(2): 115-116
Abstract:
A new chiral tetradentate ligand (S, S)-1, 5-bis (4-benzyloxazolin-2-yl-methyl)-1, 5-diazacyclo-octane 1 has been synthesized and the application of 1 as catalyst in the enantioselective addition of diethyl zinc to benzaldehyde is also described.
A new chiral tetradentate ligand (S, S)-1, 5-bis (4-benzyloxazolin-2-yl-methyl)-1, 5-diazacyclo-octane 1 has been synthesized and the application of 1 as catalyst in the enantioselective addition of diethyl zinc to benzaldehyde is also described.
2002, 13(2): 117-118
Abstract:
A new method for the synthesis of 3-N-phthaloyl homophenylalanine lactone has been developed and its mechanism was proposed
A new method for the synthesis of 3-N-phthaloyl homophenylalanine lactone has been developed and its mechanism was proposed
2002, 13(2): 119-120
Abstract:
Cholest-5-en-24-oxo-3β, 19-diacetate was synthesized starting from stigmasterol 3 via seven step reactions in 21.0% overall yield.It can be served as a key intermediate for the synthesis of many biologically active 19-hydroxylated sterols.
Cholest-5-en-24-oxo-3β, 19-diacetate was synthesized starting from stigmasterol 3 via seven step reactions in 21.0% overall yield.It can be served as a key intermediate for the synthesis of many biologically active 19-hydroxylated sterols.
2002, 13(2): 121-122
Abstract:
Alkoxysilane bearing diketone group was synthesized by hydrosilylation of 3-allyl acetylacetone.It was indicated by the 1H NMR spectrum that the C=O group does not interfere with the synthesis.
Alkoxysilane bearing diketone group was synthesized by hydrosilylation of 3-allyl acetylacetone.It was indicated by the 1H NMR spectrum that the C=O group does not interfere with the synthesis.
2002, 13(2): 123-124
Abstract:
Polyaniline doped with heteropolyacid was synthesized using solid-state synthesis method.XRD pattern showed that polyaniline molecule has highly ordered arrangement.Fluorescence property of the polyaniline materials was found.
Polyaniline doped with heteropolyacid was synthesized using solid-state synthesis method.XRD pattern showed that polyaniline molecule has highly ordered arrangement.Fluorescence property of the polyaniline materials was found.
2002, 13(2): 125-128
Abstract:
The first example of fused phosphorus heterocyclic 4-[l'-(β-bromoethyl)-4'-oxo-3'-prop yl-1', 2', 3', 4-tetrahydro-1, 3, 2-benzodiazaphosphorin-2'-sulfide]-1, 2, 3, 4, 4a, 4b, 5, 6-octahydro-6-oxo-5-propyl-3, 4b, 4a-thiazphosphaphenanthridine 4a, 2'-dioxide was synthesized in excellent yield by refluxing a mixture of 1-(2-bromoethyt)-2, 3-dihydro-3-propyl-l, 3, 2-benzodiazaphos phorin-4(1H)-one 2-oxide with carbon disulfide in benzene in the presence of triethylamine.
The first example of fused phosphorus heterocyclic 4-[l'-(β-bromoethyl)-4'-oxo-3'-prop yl-1', 2', 3', 4-tetrahydro-1, 3, 2-benzodiazaphosphorin-2'-sulfide]-1, 2, 3, 4, 4a, 4b, 5, 6-octahydro-6-oxo-5-propyl-3, 4b, 4a-thiazphosphaphenanthridine 4a, 2'-dioxide was synthesized in excellent yield by refluxing a mixture of 1-(2-bromoethyt)-2, 3-dihydro-3-propyl-l, 3, 2-benzodiazaphos phorin-4(1H)-one 2-oxide with carbon disulfide in benzene in the presence of triethylamine.
2002, 13(2): 129-132
Abstract:
A series of novel compounds 3-(2-furyl)-4-aryl-l, 2, 4-triazole-5-thiones have been synthesized.All the compounds were characterized by spectral data and elemental analysis.The preliminary biological test showed that some of them exhibited excellent plant-growth regulative acl ivities.
A series of novel compounds 3-(2-furyl)-4-aryl-l, 2, 4-triazole-5-thiones have been synthesized.All the compounds were characterized by spectral data and elemental analysis.The preliminary biological test showed that some of them exhibited excellent plant-growth regulative acl ivities.
2002, 13(2): 133-134
Abstract:
First total synthesis of (±)-hypargenin B methyl ether 2 was accomplished via a strategy of AC→ABC, in which CrO3/H2O/NaOAc/HOAc system was utilized for introducing 7-keto group in order to avoid dehydration of benzyl tertiary alcohol.
First total synthesis of (±)-hypargenin B methyl ether 2 was accomplished via a strategy of AC→ABC, in which CrO3/H2O/NaOAc/HOAc system was utilized for introducing 7-keto group in order to avoid dehydration of benzyl tertiary alcohol.
2002, 13(2): 135-138
Abstract:
Compound 1 as a key intermediate of 1, 7, 9-trideoxytaxol was synthesized in ten steps from a biosynthetically available taxane, Sinenxan A.The key steps in the synthesis were deoxygenation at C-14, allylic oxidation at C-13 and construction of the oxetane ring.
Compound 1 as a key intermediate of 1, 7, 9-trideoxytaxol was synthesized in ten steps from a biosynthetically available taxane, Sinenxan A.The key steps in the synthesis were deoxygenation at C-14, allylic oxidation at C-13 and construction of the oxetane ring.
2002, 13(2): 139-140
Abstract:
A new Eremophilanoid sesquiterpene (1) was isolated from the whole plant of Senecio oldhamianus.Its structure was elucidated as 7β, 11-epoxy-9α, 10α-epoxy-8-oxoeremophilane using spectroscopic methords and X-ray analysis.
A new Eremophilanoid sesquiterpene (1) was isolated from the whole plant of Senecio oldhamianus.Its structure was elucidated as 7β, 11-epoxy-9α, 10α-epoxy-8-oxoeremophilane using spectroscopic methords and X-ray analysis.
2002, 13(2): 141-142
Abstract:
A new abietane diterpenoid, orthosiphonol (11-methoxy-12, 14-dihydroxy-8, 11, 13-abieta trien-7-one) (1) together with known 11-hydroxysugiol (2) were isolated from Orthosiphon wulfenioides.Their structures were determined on the basis of spectroscopic evidence.
A new abietane diterpenoid, orthosiphonol (11-methoxy-12, 14-dihydroxy-8, 11, 13-abieta trien-7-one) (1) together with known 11-hydroxysugiol (2) were isolated from Orthosiphon wulfenioides.Their structures were determined on the basis of spectroscopic evidence.
2002, 13(2): 143-146
Abstract:
From the alcoholic extract of the whole plants of Serratula strangulata, two new compounds, named strangusin-A (1) and strangusin-B (2) have been isolated and their structures were established by spectroscopic method.
From the alcoholic extract of the whole plants of Serratula strangulata, two new compounds, named strangusin-A (1) and strangusin-B (2) have been isolated and their structures were established by spectroscopic method.
2002, 13(2): 147-150
Abstract:
A novel polypeptide having stimulant effect on some cell proliferation was isolated from the velvet antler (Cervus elaphus Linnaeus).The velvet antler polypeptide consists of a single chain of 32 amino acid residues.Amino acid sequence of the polypeptide was identified as:VLSAADKSNVKAAWGKVGGNAPAFGAEALLRM.
A novel polypeptide having stimulant effect on some cell proliferation was isolated from the velvet antler (Cervus elaphus Linnaeus).The velvet antler polypeptide consists of a single chain of 32 amino acid residues.Amino acid sequence of the polypeptide was identified as:VLSAADKSNVKAAWGKVGGNAPAFGAEALLRM.
2002, 13(2): 151-152
Abstract:
Several kinds of racemic naproxen ester were successfully separated on CTMB chiral stationary phase with hexane-ethanol (98:2, vol./vol.) as the mobile phase.The influence of mobile phase composition and structure of racemic naproxen ester on chiral separation was studied and the chiral recognition mechanism of CTMB was discussed.
Several kinds of racemic naproxen ester were successfully separated on CTMB chiral stationary phase with hexane-ethanol (98:2, vol./vol.) as the mobile phase.The influence of mobile phase composition and structure of racemic naproxen ester on chiral separation was studied and the chiral recognition mechanism of CTMB was discussed.
2002, 13(2): 153-156
Abstract:
Nano-gold (NG) modified glassy carbon electrodes (GCEs) were used for determination of epinephrine (EP) in the presence of high concentration ascorbic acid (AA) by cyclic voltammetry (CV).This modified electrode can not only catalytically oxidize EP and AA, but also separate the catalytic peak potentials of EP and AA by about 183.5 mV.In pH=7.0 ogisogate byffer solution, the linear range of epinephrine was 5×106~1×10-4 mol/L.
Nano-gold (NG) modified glassy carbon electrodes (GCEs) were used for determination of epinephrine (EP) in the presence of high concentration ascorbic acid (AA) by cyclic voltammetry (CV).This modified electrode can not only catalytically oxidize EP and AA, but also separate the catalytic peak potentials of EP and AA by about 183.5 mV.In pH=7.0 ogisogate byffer solution, the linear range of epinephrine was 5×106~1×10-4 mol/L.
2002, 13(2): 157-158
Abstract:
L-carnitine selective polymers were prepared by molecular imprinting using methacrylic acid as the functional monomer.The acid function of the monomer is expected to form hydrogen bond and ionic interactions with the amine function of the target molecule L-carnitine.The imprinted polymers were used as stationary phases in high-performance liquid chromatography (HPLC).It was shown that L-carnitine imprinted polymer exhibited a higher affinity to its template molecule, while the non-imprinted polymer had no affinity to the compounds tested.Racemic carnitine hydrochloride was efficiently resolved on the L-carnitine imprinted polymer, and the separation factor is 1.9.
L-carnitine selective polymers were prepared by molecular imprinting using methacrylic acid as the functional monomer.The acid function of the monomer is expected to form hydrogen bond and ionic interactions with the amine function of the target molecule L-carnitine.The imprinted polymers were used as stationary phases in high-performance liquid chromatography (HPLC).It was shown that L-carnitine imprinted polymer exhibited a higher affinity to its template molecule, while the non-imprinted polymer had no affinity to the compounds tested.Racemic carnitine hydrochloride was efficiently resolved on the L-carnitine imprinted polymer, and the separation factor is 1.9.
2002, 13(2): 159-162
Abstract:
A novel method for preparing silver nanoelectrode ensembles (SNEEs) and gold nanoelectrode ensembles (GNEEs) has been developed.Silver colloid particles were first absorbed to the gold electrode surface to form a monolayer silver colloid.N-hexadecyl mercaptan was then assembled on the electrode to form a thiol monolayer on which hydrophilic ions cannot be transfered.The SNEEs was prepared by removing thiol from silver colloid surface through applying an AC voltage with increasing frequency at 0.20 V (vs.SCE).Finally, GNEEs was obtained by immersing a SNEEs into 6 mol/L HNO3 to remove the silver colloid particles.By comparison with other methods such as template method etc., this method enjoys some advantages of lower resistance, same diameter, easy preparation, controllable size and density.
A novel method for preparing silver nanoelectrode ensembles (SNEEs) and gold nanoelectrode ensembles (GNEEs) has been developed.Silver colloid particles were first absorbed to the gold electrode surface to form a monolayer silver colloid.N-hexadecyl mercaptan was then assembled on the electrode to form a thiol monolayer on which hydrophilic ions cannot be transfered.The SNEEs was prepared by removing thiol from silver colloid surface through applying an AC voltage with increasing frequency at 0.20 V (vs.SCE).Finally, GNEEs was obtained by immersing a SNEEs into 6 mol/L HNO3 to remove the silver colloid particles.By comparison with other methods such as template method etc., this method enjoys some advantages of lower resistance, same diameter, easy preparation, controllable size and density.
2002, 13(2): 163-164
Abstract:
A new method has been developed for fabrication of copper micro-pattern by selective chemical copper deposition based on photolithographed (3-mercaptopropyl)-trimethoxysilane (MPTS) self-assembly monolayers (SAMs).As confirmed by scanning electron microscopy (SEM), Cu closely replicated the mask features.The present approach makes this technic to be cheap and may be applicable to assembly of microelectronic circuits.
A new method has been developed for fabrication of copper micro-pattern by selective chemical copper deposition based on photolithographed (3-mercaptopropyl)-trimethoxysilane (MPTS) self-assembly monolayers (SAMs).As confirmed by scanning electron microscopy (SEM), Cu closely replicated the mask features.The present approach makes this technic to be cheap and may be applicable to assembly of microelectronic circuits.
2002, 13(2): 165-166
Abstract:
The dynamic interaction process of calmodulin with an immobilized peptide melittin was investigated in real time by surface plasmon resonance spectroscopy, and dissociation constant of the complex was calculated to be 3.37×10-6mol/L.
The dynamic interaction process of calmodulin with an immobilized peptide melittin was investigated in real time by surface plasmon resonance spectroscopy, and dissociation constant of the complex was calculated to be 3.37×10-6mol/L.
2002, 13(2): 167-180
Abstract:
A series of new NIR dyes bearing 4-(4-morpholinyl) phenyl and substituted phenyl, were synthesized.The maximum absorption wavelengths of these dyes range from 928 nm to 990 nm.
A series of new NIR dyes bearing 4-(4-morpholinyl) phenyl and substituted phenyl, were synthesized.The maximum absorption wavelengths of these dyes range from 928 nm to 990 nm.
2002, 13(2): 171-174
Abstract:
The aggregating properties of Cz-C-n (n=3, 6, 10) have been investigated by means of fluorescence method in DMSO-H2O binary solvent.The measured CAC and C Φ values indicate that the aggregating tendency of the amphiphilic compounds Cz-C-n containing crown ether increases with the length of alkyl chains, similar to that of carbazole compounds with long alkyl chains.
The aggregating properties of Cz-C-n (n=3, 6, 10) have been investigated by means of fluorescence method in DMSO-H2O binary solvent.The measured CAC and C Φ values indicate that the aggregating tendency of the amphiphilic compounds Cz-C-n containing crown ether increases with the length of alkyl chains, similar to that of carbazole compounds with long alkyl chains.
2002, 13(2): 175-176
Abstract:
In the reaction of methane and carbon dioxide to C2 hydrocarbons under non-equilibrium plasma, methane conversion was decreased, but selectivity of C2 hydrocarbons was increased when using La2O3/γ-Al2O3 as catalyst.So the yield of C2 hydrocarbons was higher than using plasma alone.The synergism of La2O3/γ-Al2O3 and plasma gave methane conversion of 24.9% and C2 yield of 18.1%.The distribution of C2 hydrocarbons changed when Pd-La2O3/γ-Al2O3 was used as catalyst, the major C2 product was ethylene.
In the reaction of methane and carbon dioxide to C2 hydrocarbons under non-equilibrium plasma, methane conversion was decreased, but selectivity of C2 hydrocarbons was increased when using La2O3/γ-Al2O3 as catalyst.So the yield of C2 hydrocarbons was higher than using plasma alone.The synergism of La2O3/γ-Al2O3 and plasma gave methane conversion of 24.9% and C2 yield of 18.1%.The distribution of C2 hydrocarbons changed when Pd-La2O3/γ-Al2O3 was used as catalyst, the major C2 product was ethylene.
2002, 13(2): 177-180
Abstract:
The catalytic properties of MoOx and incorporation Ni onto the MoOx for the isomerization of heptane have been investigated under atmospheric pressure at different conditions such as different flow rate of H2, different reaction temperature etc..Compared with MoOx, the Ni addition to the MoOx markedly improved the isomerization activity of heptane by improving the reducibility of MoO3 and activation of H2 in reaction.
The catalytic properties of MoOx and incorporation Ni onto the MoOx for the isomerization of heptane have been investigated under atmospheric pressure at different conditions such as different flow rate of H2, different reaction temperature etc..Compared with MoOx, the Ni addition to the MoOx markedly improved the isomerization activity of heptane by improving the reducibility of MoO3 and activation of H2 in reaction.
2002, 13(2): 181-182
Abstract:
Ordered macroporous semiconductors CdS and ZnS with regular arrays of spherical pores have been fabricated by poly (styrene-acrylic) (PSA) colloidal crystal template.It was found that the exact three-dimensional (3D) structure of the template had been imprinted in the final material.
Ordered macroporous semiconductors CdS and ZnS with regular arrays of spherical pores have been fabricated by poly (styrene-acrylic) (PSA) colloidal crystal template.It was found that the exact three-dimensional (3D) structure of the template had been imprinted in the final material.
2002, 13(2): 183-184
Abstract:
A NaA zeolite membrane was synthesized on the surface of the stainless steel slab.The membrane was characterized by XRD and SEM.The membrane was continuous and highly intergrown.The size of NaA zeolite crystals was about 5~6 mm.
A NaA zeolite membrane was synthesized on the surface of the stainless steel slab.The membrane was characterized by XRD and SEM.The membrane was continuous and highly intergrown.The size of NaA zeolite crystals was about 5~6 mm.
2002, 13(2): 185-188
Abstract:
Mixed distannoxane dimers [ClR2SnOSnR'2Cl]2 were synthesized by the reaction of R2SnO (R=Bu, Pr) and R2SnCl2 (R=Me, Ph, Cy, Oct).The crystal structures of compound 1 and 5 show they are ladder-type dimers that contain a central planar Sn2O2 four-membered ring.Both endo-and exo-Sn atoms are five-coordinate.
Mixed distannoxane dimers [ClR2SnOSnR'2Cl]2 were synthesized by the reaction of R2SnO (R=Bu, Pr) and R2SnCl2 (R=Me, Ph, Cy, Oct).The crystal structures of compound 1 and 5 show they are ladder-type dimers that contain a central planar Sn2O2 four-membered ring.Both endo-and exo-Sn atoms are five-coordinate.
