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2001 Volume 12 Issue 1
2001, 12(1): 1-4
Abstract:
First application of optically active trans-1,2-Bis(2-aminophenyl)cyclopentane 2 for asymmetric reaction, enantioselective N-acetylation of secondary alkyl amines, is described. This acetylation with tetraacetylated 3 which was prepared from 2, gave the N-acetylamines with up to 21% ee.
First application of optically active trans-1,2-Bis(2-aminophenyl)cyclopentane 2 for asymmetric reaction, enantioselective N-acetylation of secondary alkyl amines, is described. This acetylation with tetraacetylated 3 which was prepared from 2, gave the N-acetylamines with up to 21% ee.
2001, 12(1): 5-6
Abstract:
o-Nitrophenylazide was reduced by SmI2 in anhydrous THF at room temperature to produce active intermediate 2 (samarium amide), "living" double-anion in situ which reacted smoothly with α,β-unsaturated ketones to afford 2,3-dihydro-1H-1,5-benzodiazepines in good yields under mild and neutral conditions.
o-Nitrophenylazide was reduced by SmI2 in anhydrous THF at room temperature to produce active intermediate 2 (samarium amide), "living" double-anion in situ which reacted smoothly with α,β-unsaturated ketones to afford 2,3-dihydro-1H-1,5-benzodiazepines in good yields under mild and neutral conditions.
2001, 12(1): 7-10
Abstract:
A new approach to the synthesis of 7,8,13,13a-tetrahydroisoindolo[1,2-b] [3]benzazepine 5 and 5,6,8,9,14,14a-hexahydroisoquino[1,2-b][3]benzazepine 9 and related compounds is described as using ring expansion of N-heterocycles.
A new approach to the synthesis of 7,8,13,13a-tetrahydroisoindolo[1,2-b] [3]benzazepine 5 and 5,6,8,9,14,14a-hexahydroisoquino[1,2-b][3]benzazepine 9 and related compounds is described as using ring expansion of N-heterocycles.
2001, 12(1): 11-14
Abstract:
The reaction of 7-amino-4-methyl-2(1H)-quinolone 1 and its 6-methyl derivative 2 with Vilsmeier reagent (DMF and POCl3) afforded 7-[1-aza-2-(dimethylamino)vinyl]-4-methyl-hydro-quinolin-2-one 3 and 7-[1-aza-2-(dimethylamino)vinyl]-4,6-dimethylhydroquinolin-2-one 4, respec-tively. 1H-NMR analysis in different solvents indicated that isomerism occurred due to hindered rotation around the (CH3)2N-C:N σ-bond. The rotational energy barrier of 3 was calculated.
The reaction of 7-amino-4-methyl-2(1H)-quinolone 1 and its 6-methyl derivative 2 with Vilsmeier reagent (DMF and POCl3) afforded 7-[1-aza-2-(dimethylamino)vinyl]-4-methyl-hydro-quinolin-2-one 3 and 7-[1-aza-2-(dimethylamino)vinyl]-4,6-dimethylhydroquinolin-2-one 4, respec-tively. 1H-NMR analysis in different solvents indicated that isomerism occurred due to hindered rotation around the (CH3)2N-C:N σ-bond. The rotational energy barrier of 3 was calculated.
2001, 12(1): 15-18
Abstract:
In present paper, the 2,3-diaryl-butadiene analogues were synthesized as anti-cancer agents. The structures were confirmed by 1HNMR and elemental analysis.
In present paper, the 2,3-diaryl-butadiene analogues were synthesized as anti-cancer agents. The structures were confirmed by 1HNMR and elemental analysis.
2001, 12(1): 19-20
Abstract:
19-Nor-1α, 25-dihydroxy-22-oxo-vitamin D3 4 was synthesized by the coupling of known compound 5 and the A-ring phosphine oxide 6 followed by deprotection of the hydroxy functions.
19-Nor-1α, 25-dihydroxy-22-oxo-vitamin D3 4 was synthesized by the coupling of known compound 5 and the A-ring phosphine oxide 6 followed by deprotection of the hydroxy functions.
2001, 12(1): 21-24
Abstract:
A short and efficient procedure for introduction of tertiary hydroxyl to C-11 of eudesmanolide based on the rearrangement-oxidation of the exocylic double bond has been developed, which is synthetically valuable for a series of natural eudesmanolide sesquiterpenoids containing the 11,12-diol.
A short and efficient procedure for introduction of tertiary hydroxyl to C-11 of eudesmanolide based on the rearrangement-oxidation of the exocylic double bond has been developed, which is synthetically valuable for a series of natural eudesmanolide sesquiterpenoids containing the 11,12-diol.
2001, 12(1): 25-26
Abstract:
We have developed an alternative route to synthesize Tn antigen. The synthetic product was characterized by IR, 1H-NMR and elemental analysis.
We have developed an alternative route to synthesize Tn antigen. The synthetic product was characterized by IR, 1H-NMR and elemental analysis.
2001, 12(1): 27-30
Abstract:
A series of novel organic compounds named as CSPI, DPASPI, PSPI DEASPI and HEASPI respectively, with large two-photon absorption has been synthesized and their structures have been determined by 1HNMR and elemental analysis. The highest two-photon pumped (TPP) output /input efficiency is as high as 13.4% for PSPI in DMF with d0=0.03 mol/L and the effective two-photon absorption cross section is 8.8×10-48 cm4·s/photon for DPASPI in DMF with d0=0.05mol/L.
A series of novel organic compounds named as CSPI, DPASPI, PSPI DEASPI and HEASPI respectively, with large two-photon absorption has been synthesized and their structures have been determined by 1HNMR and elemental analysis. The highest two-photon pumped (TPP) output /input efficiency is as high as 13.4% for PSPI in DMF with d0=0.03 mol/L and the effective two-photon absorption cross section is 8.8×10-48 cm4·s/photon for DPASPI in DMF with d0=0.05mol/L.
2001, 12(1): 31-34
Abstract:
Five new aza-crown ethers have been prepared by the condensation of 2,6-bis[(2-formylphenyl)oxymethyl] pyridine with different diamino compounds in hot methanol, the bis-Schiff bases without isolation were reduced with NaBH4 to afford the corresponding aza-crown ethers. The liquid membrane transport of alkali cations using the five new macrocycles as the ion-carriers was also studied.
Five new aza-crown ethers have been prepared by the condensation of 2,6-bis[(2-formylphenyl)oxymethyl] pyridine with different diamino compounds in hot methanol, the bis-Schiff bases without isolation were reduced with NaBH4 to afford the corresponding aza-crown ethers. The liquid membrane transport of alkali cations using the five new macrocycles as the ion-carriers was also studied.
2001, 12(1): 35-38
Abstract:
The reactive properties of 1,3-dichloro-1,1,3,3-tetraphenyldisilazane (DCTPS) with water, methanol, phenylamine and lithium salt of hexamethylcyclotrisilazane (D3Nli) were investigated, and four new derivatives were obtained.
The reactive properties of 1,3-dichloro-1,1,3,3-tetraphenyldisilazane (DCTPS) with water, methanol, phenylamine and lithium salt of hexamethylcyclotrisilazane (D3Nli) were investigated, and four new derivatives were obtained.
2001, 12(1): 39-40
Abstract:
β-Bromovinyl tellurides are new difuctional reagents which undergo palladium-catalyzed cross-coupling reaction with alkenes to give conjugated dienyl tellurides.
β-Bromovinyl tellurides are new difuctional reagents which undergo palladium-catalyzed cross-coupling reaction with alkenes to give conjugated dienyl tellurides.
2001, 12(1): 41-42
Abstract:
The ring opening polymerization of 2,2-dimethyltrimethylene carbonate (DTC) initiated by single component of tris(2,6-di-tert-butyl-4-methylphenoxo) lanthanide (Ln(OAr)3) is reported. The initiators are highly active to the polymerization and give high molecular weight polymers. 1HNMR spectra and DSC measurement suggest the polymerization is free of decarboxylation. Mechanism study shows that the monomer insertion is via the break of acyl-oxygen bond of DTC.
The ring opening polymerization of 2,2-dimethyltrimethylene carbonate (DTC) initiated by single component of tris(2,6-di-tert-butyl-4-methylphenoxo) lanthanide (Ln(OAr)3) is reported. The initiators are highly active to the polymerization and give high molecular weight polymers. 1HNMR spectra and DSC measurement suggest the polymerization is free of decarboxylation. Mechanism study shows that the monomer insertion is via the break of acyl-oxygen bond of DTC.
2001, 12(1): 43-46
Abstract:
The partial oxidation of butane (POB) to syngas over nickel supported catalysts was first investigated with a flow-reactor, TG and UVRRS. The NiO/γ-Al2O3 is the most suitable for the POB among NiO/γ-Al2O3, NiO/MgO and NiO/SiO2. And the reaction performance of the NiO/γ-Al2O3 shows little difference from those of the nickel supported catalysts modified by alkali metal oxide and rare-earth metal oxide. However, modification with Li2O and La2O3 can suppress carbon-deposition of the NiO/γ-Al2O3, which contains graphite-like species during the POB reaction.
The partial oxidation of butane (POB) to syngas over nickel supported catalysts was first investigated with a flow-reactor, TG and UVRRS. The NiO/γ-Al2O3 is the most suitable for the POB among NiO/γ-Al2O3, NiO/MgO and NiO/SiO2. And the reaction performance of the NiO/γ-Al2O3 shows little difference from those of the nickel supported catalysts modified by alkali metal oxide and rare-earth metal oxide. However, modification with Li2O and La2O3 can suppress carbon-deposition of the NiO/γ-Al2O3, which contains graphite-like species during the POB reaction.
2001, 12(1): 47-48
Abstract:
A new phenolic compound, thamnolin (1), was isolated from the extract of Thamnolia vermicularis. Its structure was determined as 6-tricosyl-2,4-dimethoxy-phenol by spectral methods.
A new phenolic compound, thamnolin (1), was isolated from the extract of Thamnolia vermicularis. Its structure was determined as 6-tricosyl-2,4-dimethoxy-phenol by spectral methods.
2001, 12(1): 49-50
Abstract:
A new special flavone, named desmosdumotin B, was isolated from the roots of D. dumosus and its chemical structure identified as 5-hydroxy-7-one-6,8,8-trimethylflavone by spectral analysis and X-ray.
A new special flavone, named desmosdumotin B, was isolated from the roots of D. dumosus and its chemical structure identified as 5-hydroxy-7-one-6,8,8-trimethylflavone by spectral analysis and X-ray.
2001, 12(1): 51-54
Abstract:
Five new diterpenoids isolated from Siegesbeckia pubescens, pubesides A~E, were established as ent-2α,15,16-trihydroxypimar-8(14)-en-2-O-β-D-glucopyranoside (1), ent-15,16,19-trihydroxypimar-8(14)-en-19-O-β-D-glucopyranoside (2), b-D-glucopyranosyl-ent-15,16-dihydroxypimar-8(14)-en-19-oiclate (3), ent-2-oxo-15,16,19-trihydroxypimar-8(14)-en-19-O-β-D-gluco-pyranoside (4), ent-2-oxo-15,16,19-trihydroxypimar-8(14)-en-19-O-β-D-glucopyranoside-15,16-acetonide (5) by 1D and 2D NMR techniques.
Five new diterpenoids isolated from Siegesbeckia pubescens, pubesides A~E, were established as ent-2α,15,16-trihydroxypimar-8(14)-en-2-O-β-D-glucopyranoside (1), ent-15,16,19-trihydroxypimar-8(14)-en-19-O-β-D-glucopyranoside (2), b-D-glucopyranosyl-ent-15,16-dihydroxypimar-8(14)-en-19-oiclate (3), ent-2-oxo-15,16,19-trihydroxypimar-8(14)-en-19-O-β-D-gluco-pyranoside (4), ent-2-oxo-15,16,19-trihydroxypimar-8(14)-en-19-O-β-D-glucopyranoside-15,16-acetonide (5) by 1D and 2D NMR techniques.
2001, 12(1): 55-58
Abstract:
A new 30-nortriterpenoid glycopside, 3-O-α-L-arabinopyranosyl-30-norhederagenin 28-O-α-L-rhamnopyranosyl(1→4)-β-D-glucopyranosyl (1→6)-β-D-glucopyranoside 1, named sinofoside A was isolated from Sinofranchetia chinensis. Its structrue was elucidadated by spectra FAB-MS, 2D-NMR including 1H-1H COSY, 1H-13C COSY, TOSCY, HMBC and NOESY techniques.
A new 30-nortriterpenoid glycopside, 3-O-α-L-arabinopyranosyl-30-norhederagenin 28-O-α-L-rhamnopyranosyl(1→4)-β-D-glucopyranosyl (1→6)-β-D-glucopyranoside 1, named sinofoside A was isolated from Sinofranchetia chinensis. Its structrue was elucidadated by spectra FAB-MS, 2D-NMR including 1H-1H COSY, 1H-13C COSY, TOSCY, HMBC and NOESY techniques.
2001, 12(1): 59-62
Abstract:
Notoginsenoside R10, a novel hexanordammarane glycoside was isolated from the roots of Panax nototginseng, as a minor constituent. Its structure was determined as 6-O-(β-D-glucopyranosyl)-3β,6α,12β-trihydroxy-22,23,24,25,26,27-hexanordammaran-20-one(1), by means of spectroscopic methods.
Notoginsenoside R10, a novel hexanordammarane glycoside was isolated from the roots of Panax nototginseng, as a minor constituent. Its structure was determined as 6-O-(β-D-glucopyranosyl)-3β,6α,12β-trihydroxy-22,23,24,25,26,27-hexanordammaran-20-one(1), by means of spectroscopic methods.
2001, 12(1): 63-66
Abstract:
From the barks of Taxus yunnanensis, a new paclitaxel-related compound, 7-xylosyl-taxol D (1), and three new 11(15→1)-abeotaxoids, taxuyunnanines P-R (2-4) have been isolated. Their structures were determined on the basis of spectral methods. Taxuyunnanines P-R are a rare type of naturally occurring abeotaxoids with an opened D-ring system.
From the barks of Taxus yunnanensis, a new paclitaxel-related compound, 7-xylosyl-taxol D (1), and three new 11(15→1)-abeotaxoids, taxuyunnanines P-R (2-4) have been isolated. Their structures were determined on the basis of spectral methods. Taxuyunnanines P-R are a rare type of naturally occurring abeotaxoids with an opened D-ring system.
2001, 12(1): 67-68
Abstract:
Chemical investigation on the ethanol extract from the roots of Spiraea japonica var. acuta resulted in the isolation of two new diterpene alkaloids named spiratines A and B (1-2), respectively.
Chemical investigation on the ethanol extract from the roots of Spiraea japonica var. acuta resulted in the isolation of two new diterpene alkaloids named spiratines A and B (1-2), respectively.
2001, 12(1): 69-70
Abstract:
A new kind of hydrazone (I) diastereoisomers was prepared with enantiomeric hydazide (Ⅱ) and chiral cluster (Ⅲ), which was characterized by HMBC. Unfortunately, the mixture could not be separated into pure diastereoisomer. This could be a direction to separate the racemic chiral clusters.
A new kind of hydrazone (I) diastereoisomers was prepared with enantiomeric hydazide (Ⅱ) and chiral cluster (Ⅲ), which was characterized by HMBC. Unfortunately, the mixture could not be separated into pure diastereoisomer. This could be a direction to separate the racemic chiral clusters.
2001, 12(1): 71-72
Abstract:
A novel reactive resin as active support was synthesized by an improved method based on seed swelling and surface coating polymerization. The resin is monosized beads with inner nucleus of cross-linked polymer and surface layer of copolymer containing epoxy groups. The physico-chemical structures of beads were characterized.
A novel reactive resin as active support was synthesized by an improved method based on seed swelling and surface coating polymerization. The resin is monosized beads with inner nucleus of cross-linked polymer and surface layer of copolymer containing epoxy groups. The physico-chemical structures of beads were characterized.
2001, 12(1): 73-74
Abstract:
A new electrode was prepared by using Pd implanted into nano-crystalline TiO2 and the character of photo-electrochemistry of implanted electrodes was investigated. The energy band structure of nano-crystalline TiO2 has not changed after implantation with Pd. The photo-current (iph) of palladium implanted TiO2 nano-crystalline electrode is larger than that of pure TiO2 nano-crystalline electrode.
A new electrode was prepared by using Pd implanted into nano-crystalline TiO2 and the character of photo-electrochemistry of implanted electrodes was investigated. The energy band structure of nano-crystalline TiO2 has not changed after implantation with Pd. The photo-current (iph) of palladium implanted TiO2 nano-crystalline electrode is larger than that of pure TiO2 nano-crystalline electrode.
2001, 12(1): 75-78
Abstract:
The static O-H bond parameters including O-H bond length, O-H charge difference, O-H Mulliken population and O-H bond stretching force constant (k) for 17 phenols were calculated by ab initio method HF/6-31G**. In combination with the O-H bond dissociation enthalpies (BDE) of the phenols determined by experiment, it was found that there were poor correlationships between the static O-H bond parameters and O-H BDE. Considering the good correlationship between O-H BDE and logarithm of free radical scavenging rate constant for phenolic antioxidant, it is reasonable to believe that the ineffectiveness of static O-H bond parameters in characterizing antioxidant activity arises from the fact that they cannot measure the O-H BDE.
The static O-H bond parameters including O-H bond length, O-H charge difference, O-H Mulliken population and O-H bond stretching force constant (k) for 17 phenols were calculated by ab initio method HF/6-31G**. In combination with the O-H bond dissociation enthalpies (BDE) of the phenols determined by experiment, it was found that there were poor correlationships between the static O-H bond parameters and O-H BDE. Considering the good correlationship between O-H BDE and logarithm of free radical scavenging rate constant for phenolic antioxidant, it is reasonable to believe that the ineffectiveness of static O-H bond parameters in characterizing antioxidant activity arises from the fact that they cannot measure the O-H BDE.
2001, 12(1): 79-80
Abstract:
An apparatus for measuring the enthalpy of solution of solids in supercritical fluids (SCFs) was constructed. The enthalpy of solution (ΔH) of naphthalene in supercritical (SC) CO2 was measured at 308.15 K in the pressure range from 8~11 MPa. It was found that ΔH was negative in the pressure range from 8 to 10 MPa, and the absolute value of ΔH decreases with increasing pressure. However, ΔH became positive at the pressures higher than 10 MPa. This unusual phenomenon can be explained by clustering between CO2 and naphthalene.
An apparatus for measuring the enthalpy of solution of solids in supercritical fluids (SCFs) was constructed. The enthalpy of solution (ΔH) of naphthalene in supercritical (SC) CO2 was measured at 308.15 K in the pressure range from 8~11 MPa. It was found that ΔH was negative in the pressure range from 8 to 10 MPa, and the absolute value of ΔH decreases with increasing pressure. However, ΔH became positive at the pressures higher than 10 MPa. This unusual phenomenon can be explained by clustering between CO2 and naphthalene.
2001, 12(1): 81-82
Abstract:
The densities of n-pentane, methane-n-pentane, propane-n-pentane, n-heptane-n-pentane, and n-decane-n-pentane binary mixtures were determined at 476.5K in the pressure range from 2 to 5 MPa. The partial molar volumes of the solutes in n-pentane were calculated using the density data. It was found that the partial molar volumes of methane and propane are positive. while those of n-heptane and n-decane are negative.
The densities of n-pentane, methane-n-pentane, propane-n-pentane, n-heptane-n-pentane, and n-decane-n-pentane binary mixtures were determined at 476.5K in the pressure range from 2 to 5 MPa. The partial molar volumes of the solutes in n-pentane were calculated using the density data. It was found that the partial molar volumes of methane and propane are positive. while those of n-heptane and n-decane are negative.
2001, 12(1): 83-86
Abstract:
The decomposition of NO has been studied in a steady flow reactor on fresh carbon nanotubes (CNTs), purified CNTs, Rh/p-CNTs and Rh/γ-Al2O3 between 573 K and 973 K. NO decomposition at 573 K was initially complete over a reduced surface. The amount of NO absorption increased at temperature below 773 K. 100% NO conversion and more than 100% N2 activity was achieved at 973 K for 150 min on p-CNTs and f-CNTs.
The decomposition of NO has been studied in a steady flow reactor on fresh carbon nanotubes (CNTs), purified CNTs, Rh/p-CNTs and Rh/γ-Al2O3 between 573 K and 973 K. NO decomposition at 573 K was initially complete over a reduced surface. The amount of NO absorption increased at temperature below 773 K. 100% NO conversion and more than 100% N2 activity was achieved at 973 K for 150 min on p-CNTs and f-CNTs.
2001, 12(1): 87-90
Abstract:
In this paper, α-amylase organized monolayer was assembled on the surface of the PET-CO2-substrate in different conditions. The different topography of the α-amylase/PET monolayer was obtained by AFM in tapping mode.
In this paper, α-amylase organized monolayer was assembled on the surface of the PET-CO2-substrate in different conditions. The different topography of the α-amylase/PET monolayer was obtained by AFM in tapping mode.
2001, 12(1): 91-94
Abstract:
Amphiphilic molecules can form into different structures, such as micelle, microemulsion, vesicle, liposome, liquid crystals, and so on by self-associating. The Dielectric Spectroscopy (DS) method has been applied to the systems of micelle and microemulsion successfully. For the first time the author put the method to the system of vesicle of CTAB/SDBS. The experiments show clear dielectric relaxation and the results were discussed primarily.
Amphiphilic molecules can form into different structures, such as micelle, microemulsion, vesicle, liposome, liquid crystals, and so on by self-associating. The Dielectric Spectroscopy (DS) method has been applied to the systems of micelle and microemulsion successfully. For the first time the author put the method to the system of vesicle of CTAB/SDBS. The experiments show clear dielectric relaxation and the results were discussed primarily.
