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2003 Volume 20 Issue 3
2003, 20(3): 205-209
Abstract:
Salicylaldehyde-1H-benzotriazol-1-acetyl hydrazone (C15H13N5O2, H2L, SBTH) and its seven complexes with lanthanide perchlorates RE(HL)2ClO4(RE=Pr, Nd, Sm, Eu,Gd, Tb and Dy) have been synthesized and confirmed by elemental analysis, chemical analysis and molar conductivity measurement. The IR, UV and 1H NMR results indicate that the SBTH is bonded with RE3+ via the carbonyl and phenol oxygen and imidogen nitrogen, forming a pentacyclic and hexacyclic tridentate complex.The complexes show a certain antibacterial activity against leaf mold, bacilli and actinomyceto.
Salicylaldehyde-1H-benzotriazol-1-acetyl hydrazone (C15H13N5O2, H2L, SBTH) and its seven complexes with lanthanide perchlorates RE(HL)2ClO4(RE=Pr, Nd, Sm, Eu,Gd, Tb and Dy) have been synthesized and confirmed by elemental analysis, chemical analysis and molar conductivity measurement. The IR, UV and 1H NMR results indicate that the SBTH is bonded with RE3+ via the carbonyl and phenol oxygen and imidogen nitrogen, forming a pentacyclic and hexacyclic tridentate complex.The complexes show a certain antibacterial activity against leaf mold, bacilli and actinomyceto.
2003, 20(3): 210-214
Abstract:
The rheological properties of acrylate copolymer emulsions modified by organosilicone have been investigated by using a rotating viscometer.It was found that the apparent viscosity of the emulsions decreased with increase of the amounts of Si-1.The viscosity values of organosilicone-modified acrylate emuslions were near to that of pure acrylates when ω(Si-1)=24% emulsion. And the high the solid content the high the viscosity of the emulsions.The emulsions containing polymerizable emulsifiers had rather lower viscosity and better stability.
The rheological properties of acrylate copolymer emulsions modified by organosilicone have been investigated by using a rotating viscometer.It was found that the apparent viscosity of the emulsions decreased with increase of the amounts of Si-1.The viscosity values of organosilicone-modified acrylate emuslions were near to that of pure acrylates when ω(Si-1)=24% emulsion. And the high the solid content the high the viscosity of the emulsions.The emulsions containing polymerizable emulsifiers had rather lower viscosity and better stability.
2003, 20(3): 215-218
Abstract:
The inclusion phenomena occurred between β-cyclodextrin (β-CD) and eight cyanine dyes has been investigated by UV-vis spectrometry.The results showed that presence of β-CD, in general, can increase the absorbance and photostability of cyanine dyes in aq. solution and for the same series of asymmetric monomethine thiazine dyes the dye with greater substituents attached in aromatic ring reveals the most enhancement in photostability.
The inclusion phenomena occurred between β-cyclodextrin (β-CD) and eight cyanine dyes has been investigated by UV-vis spectrometry.The results showed that presence of β-CD, in general, can increase the absorbance and photostability of cyanine dyes in aq. solution and for the same series of asymmetric monomethine thiazine dyes the dye with greater substituents attached in aromatic ring reveals the most enhancement in photostability.
2003, 20(3): 219-222
Abstract:
Esterifications of benzoic acid with alcohols by using Yb(N(SO2CF3)2)3, abbr. Yb(NTf2)3 as a Lew is acid catalyst have been investigated as function of reaction time, reaction temperature, catalyst dosage, solvents and alcohol acid molar ratio. Under the optimum conditions:Yb(NTf2)3 8%, molar ratio of alcohol to acid 7:1, reflux time 6 h, the yield of ethyl benzoate was over 99%.In the esterification reactions of benzoic acid with different structure alcohols Yb(NTf2)3 demonstrated much higher catalytic activity than traditional catalysts such as concentrated H2SO4, FeCl3, SnCl2, and even Yb(OTf)3.
Esterifications of benzoic acid with alcohols by using Yb(N(SO2CF3)2)3, abbr. Yb(NTf2)3 as a Lew is acid catalyst have been investigated as function of reaction time, reaction temperature, catalyst dosage, solvents and alcohol acid molar ratio. Under the optimum conditions:Yb(NTf2)3 8%, molar ratio of alcohol to acid 7:1, reflux time 6 h, the yield of ethyl benzoate was over 99%.In the esterification reactions of benzoic acid with different structure alcohols Yb(NTf2)3 demonstrated much higher catalytic activity than traditional catalysts such as concentrated H2SO4, FeCl3, SnCl2, and even Yb(OTf)3.
2003, 20(3): 223-227
Abstract:
A porous spherical hydroxyapatite (HA) ceramic biomaterial has been prepared directly by a simple chemical synthetic method followed by treatment with chitosan solution and calcination. The synthesized HA material of high purity consisted of a unique normal HA structure as confirmed by XRD and IR measurements.The size of fine spherical HA with most inner ducts linked up to each other for fresh bone to develop was well distributed between 400~700 μm by SEM observation. The mass ratio of Ca and P was about 1.67, close to that in human bone. The porous HA coated by polyactic acid (PLA) has been explored for drug delivery material using serum albumin as a model protein. A good result was obtained.
A porous spherical hydroxyapatite (HA) ceramic biomaterial has been prepared directly by a simple chemical synthetic method followed by treatment with chitosan solution and calcination. The synthesized HA material of high purity consisted of a unique normal HA structure as confirmed by XRD and IR measurements.The size of fine spherical HA with most inner ducts linked up to each other for fresh bone to develop was well distributed between 400~700 μm by SEM observation. The mass ratio of Ca and P was about 1.67, close to that in human bone. The porous HA coated by polyactic acid (PLA) has been explored for drug delivery material using serum albumin as a model protein. A good result was obtained.
2003, 20(3): 228-232
Abstract:
Methyl orange (MO) doped SiO2 xerogels derived from tetraethyl orthosilicate (TEOS) and modified with cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulfate (SDS) and stearic acid (SA) respectively, were prepared. FTIR and TG analyses were used to characterize the xerogels. The color change and leaching behavior of MO in the xerogels were investigated. The experimental results show that MO in the xerogels has no definite pH value color change. The color change pH values of MO in the xerogel doped with CTAB shift to low pH values, and are lower than those of MO in the other surfactant doped xerogels. The xerogel doped with SDS shows the highest leaching rate of MO. The leaching rates in solutions of different pH values after 7 days are all higher than 30%. The leaching rate of MO in the xerogel doped with CTAB is the lowest, and the leaching rate in acidic and neutral solutions after 7 days is lower than 0.05%. The results have been discussed.
Methyl orange (MO) doped SiO2 xerogels derived from tetraethyl orthosilicate (TEOS) and modified with cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulfate (SDS) and stearic acid (SA) respectively, were prepared. FTIR and TG analyses were used to characterize the xerogels. The color change and leaching behavior of MO in the xerogels were investigated. The experimental results show that MO in the xerogels has no definite pH value color change. The color change pH values of MO in the xerogel doped with CTAB shift to low pH values, and are lower than those of MO in the other surfactant doped xerogels. The xerogel doped with SDS shows the highest leaching rate of MO. The leaching rates in solutions of different pH values after 7 days are all higher than 30%. The leaching rate of MO in the xerogel doped with CTAB is the lowest, and the leaching rate in acidic and neutral solutions after 7 days is lower than 0.05%. The results have been discussed.
2003, 20(3): 233-237
Abstract:
The influence of water-to-surfactant-ratio R on the composition and size distribution of the Ni-Fe composite nanoparticles prepared by a microemulsion method has been investigated. The results showed that the size and composition of nanoparticles would change with R value. When R<18 the Ni-Fe alloy would be obtained. It was found that the coereivity values of composite Ni-Fe particles were reduced with Ni-Fe particle size. The Ni-Fe nanoparticles had specific saturation magnetization intensity of 50.02×10-3~217.68×10-3 A/(m·g); coerevity values of 2.388~10.030 kA/m; and remanent magnetism of 28.28×10-3~37.7×10-3 A/(m·g).
The influence of water-to-surfactant-ratio R on the composition and size distribution of the Ni-Fe composite nanoparticles prepared by a microemulsion method has been investigated. The results showed that the size and composition of nanoparticles would change with R value. When R<18 the Ni-Fe alloy would be obtained. It was found that the coereivity values of composite Ni-Fe particles were reduced with Ni-Fe particle size. The Ni-Fe nanoparticles had specific saturation magnetization intensity of 50.02×10-3~217.68×10-3 A/(m·g); coerevity values of 2.388~10.030 kA/m; and remanent magnetism of 28.28×10-3~37.7×10-3 A/(m·g).
2003, 20(3): 238-241
Abstract:
A novel monomer 2,6-diphenoxybenzonitrile (DPOBN) was prepared by condensation of 2,6-dichlorobenzonitrile with phenol in NMP in the presence of KOH and K2CO3. A poly(arylether ether ketone ketone)(PEEKK) containing cyano groups was synthesized by low temperature solution polycondensation of 2,6-diphenoxybenzonitrile with terephthaloyl dichloride (TPC) in 1,2-dichloroethane and in the presence of AlCl3 and NMP. Effects of the molar ratio of DPOBN to TPC and the amounts of AlCl3 and NMP on polycondensation were investigated. IR, DSC, TG, WAXD techniques were used to characterize the polymer. The results showed that the Tg of the polymer was 180℃, 24℃ more than that of the PEKK(Tg=156℃) and the polymer was noncrystalline. The polymer has an excellent heat-res istance(Td=495℃) and good solubility in DMF, NMP and DMSO.
A novel monomer 2,6-diphenoxybenzonitrile (DPOBN) was prepared by condensation of 2,6-dichlorobenzonitrile with phenol in NMP in the presence of KOH and K2CO3. A poly(arylether ether ketone ketone)(PEEKK) containing cyano groups was synthesized by low temperature solution polycondensation of 2,6-diphenoxybenzonitrile with terephthaloyl dichloride (TPC) in 1,2-dichloroethane and in the presence of AlCl3 and NMP. Effects of the molar ratio of DPOBN to TPC and the amounts of AlCl3 and NMP on polycondensation were investigated. IR, DSC, TG, WAXD techniques were used to characterize the polymer. The results showed that the Tg of the polymer was 180℃, 24℃ more than that of the PEKK(Tg=156℃) and the polymer was noncrystalline. The polymer has an excellent heat-res istance(Td=495℃) and good solubility in DMF, NMP and DMSO.
2003, 20(3): 242-245
Abstract:
Erbium oxide was added to Bi2O3-MoO3 mixed oxides catalyst(Mo-Bi-O) via coprecipitation. Reaction temperature, concentration of isobutene in air and ratio of Er2O3 in the Mo-Bi-O catalysts were studied in a fixed bed reactor. The results showed that conversion of isobutene and selectivity for methacrolein was improved when erbium oxide was added in the catalyst. The maximum yield of methacrolein was obtained when proportion of erbium reached 15%. XRD patterns of the catalyst samples revealed that the main component of the Mo-Bi-O catalyst with added erbium is Er2Mo3O12.
Erbium oxide was added to Bi2O3-MoO3 mixed oxides catalyst(Mo-Bi-O) via coprecipitation. Reaction temperature, concentration of isobutene in air and ratio of Er2O3 in the Mo-Bi-O catalysts were studied in a fixed bed reactor. The results showed that conversion of isobutene and selectivity for methacrolein was improved when erbium oxide was added in the catalyst. The maximum yield of methacrolein was obtained when proportion of erbium reached 15%. XRD patterns of the catalyst samples revealed that the main component of the Mo-Bi-O catalyst with added erbium is Er2Mo3O12.
2003, 20(3): 246-249
Abstract:
Soybean phospholipids were separated into phospholipids on a semi-preparative silica gel column using HPLC. Phosphatidylcholine(PC), phosphatidylethanolamine(PE) and phosphatidylinositol(PI) fractions were collected. Their molecular species compositions were analysed on a revers phase Prodigy ODS(3) column and a gradient elution program performed with chloroform-methanol-acetonitrile-water as a flow phase. Phosphatidylcholine, phosphatidy lethanolamine and phosphatidylinositol were separated into 11, 9 and 10 molecular species respectively. The molecular species identities were assigned from fatty acid compositions determined by gas chromatography (GC). The method has advantages of simplicity and availability of solvents.
Soybean phospholipids were separated into phospholipids on a semi-preparative silica gel column using HPLC. Phosphatidylcholine(PC), phosphatidylethanolamine(PE) and phosphatidylinositol(PI) fractions were collected. Their molecular species compositions were analysed on a revers phase Prodigy ODS(3) column and a gradient elution program performed with chloroform-methanol-acetonitrile-water as a flow phase. Phosphatidylcholine, phosphatidy lethanolamine and phosphatidylinositol were separated into 11, 9 and 10 molecular species respectively. The molecular species identities were assigned from fatty acid compositions determined by gas chromatography (GC). The method has advantages of simplicity and availability of solvents.
2003, 20(3): 250-253
Abstract:
The title complex was synthesized and its crystal structure was determined by X-ray diffractometry. The result indicates that the Mn(Ⅱ) complex is six-coord inated (two PMBP and two EtOH) with a distorted octahedral structure and chemical formula Mn(PMBP)2(EtOH)2. The crystal is monoclinic, space group P2(1)/n, a=0.9949(4) nm, b=1.6295(6) nm, c=2.2111(8) nm, β=100.976(7)°. The preliminary anti-bacterial activity tests showed the complex processes an inhibitory action to Escherichia Coli and Staphylococcus aureus.
The title complex was synthesized and its crystal structure was determined by X-ray diffractometry. The result indicates that the Mn(Ⅱ) complex is six-coord inated (two PMBP and two EtOH) with a distorted octahedral structure and chemical formula Mn(PMBP)2(EtOH)2. The crystal is monoclinic, space group P2(1)/n, a=0.9949(4) nm, b=1.6295(6) nm, c=2.2111(8) nm, β=100.976(7)°. The preliminary anti-bacterial activity tests showed the complex processes an inhibitory action to Escherichia Coli and Staphylococcus aureus.
2003, 20(3): 254-257
Abstract:
A fumed silica-supported sulfur, phosphine mixed bidentate palladium complex (‘Si’-S,P-Pd) has been synthesized by reaction of poly-4-thia-6-diphenylpho sphinohexylsiloxane(‘Si’-S,P) with palladium chloride in acetone at 60℃ for 72 h and characterized by elemental analysis and X-ray photoelectron spectrometry. A possible structure pattern of the polymeric palladium complex has been proposed. The results show that in the presence of a catalytic amount of the title complex the amidation and the butoxycarbonylation of aryl halides under atmospheric pressure of carbon monoxide (Heck carbonylation) proceed smoothly to give the corresponding substituted N-phenylbenzamides and butyl benzoates in good yields. The reactivities of aryl iodides are obviously higher than that of corresponding aryl bromides. The polymeric palladium catalyst can be regenerated and reused without serious loss of its activity.
A fumed silica-supported sulfur, phosphine mixed bidentate palladium complex (‘Si’-S,P-Pd) has been synthesized by reaction of poly-4-thia-6-diphenylpho sphinohexylsiloxane(‘Si’-S,P) with palladium chloride in acetone at 60℃ for 72 h and characterized by elemental analysis and X-ray photoelectron spectrometry. A possible structure pattern of the polymeric palladium complex has been proposed. The results show that in the presence of a catalytic amount of the title complex the amidation and the butoxycarbonylation of aryl halides under atmospheric pressure of carbon monoxide (Heck carbonylation) proceed smoothly to give the corresponding substituted N-phenylbenzamides and butyl benzoates in good yields. The reactivities of aryl iodides are obviously higher than that of corresponding aryl bromides. The polymeric palladium catalyst can be regenerated and reused without serious loss of its activity.
2003, 20(3): 258-261
Abstract:
The Pb(Ⅱ) ions have been separated by a flotation system consisted of ammonium sulfate, potassium iodide and ethyl vielot(EV). The results show that ternary ion-association precipitates (PbI3-)·(EV+) and (PbI42-)·(EV+)2 are formed. In the presence of 0.1 g/mL (NH4)2SO4, the precipitates floated on the surface of water phase can be easily separated by water. Thus Pb(Ⅱ) can be completely separated from Zn(Ⅱ), Mn(Ⅱ), Fe(Ⅲ), Co(Ⅱ), Al(Ⅲ) and Ni(Ⅱ) in aqueous solution of pH=1.0~4.0.
The Pb(Ⅱ) ions have been separated by a flotation system consisted of ammonium sulfate, potassium iodide and ethyl vielot(EV). The results show that ternary ion-association precipitates (PbI3-)·(EV+) and (PbI42-)·(EV+)2 are formed. In the presence of 0.1 g/mL (NH4)2SO4, the precipitates floated on the surface of water phase can be easily separated by water. Thus Pb(Ⅱ) can be completely separated from Zn(Ⅱ), Mn(Ⅱ), Fe(Ⅲ), Co(Ⅱ), Al(Ⅲ) and Ni(Ⅱ) in aqueous solution of pH=1.0~4.0.
2003, 20(3): 262-265
Abstract:
Five solid complexes of Schiff base KC14H12NO4 (KL) derived from furfural and L-tyrosine with rare earth nitrates have been synthesized and characterized by elemental analysis, IR, UV and molar conductance measurement. The composition of the complexes were confirmed to be [LnL(NO3)(H2O)2]NO3·xH2O (Ln=Gd,Dy,Nd,Er,La,Sm, x=0~2). The thermodecomposition kinetics of Er(Ⅲ) complex at initial decomposition stage under non-isothermal condition was studied. The kinetic equation appeared to be:dα/dt=A·e-E/RT·(1-α)2.
Five solid complexes of Schiff base KC14H12NO4 (KL) derived from furfural and L-tyrosine with rare earth nitrates have been synthesized and characterized by elemental analysis, IR, UV and molar conductance measurement. The composition of the complexes were confirmed to be [LnL(NO3)(H2O)2]NO3·xH2O (Ln=Gd,Dy,Nd,Er,La,Sm, x=0~2). The thermodecomposition kinetics of Er(Ⅲ) complex at initial decomposition stage under non-isothermal condition was studied. The kinetic equation appeared to be:dα/dt=A·e-E/RT·(1-α)2.
2003, 20(3): 266-268
Abstract:
The cationic polyurethane/CeO2 nanocomposite dispersion has been synthesized by adding ceria organosol to pre-polymer of polyurethane and then adding neutralization reagent and water to give an emulsion. FTIR analysis shows blue shift of the absorpsion band of CeO2. TEM micrograph shows that CeO2 nano-particles are uniformly dispersed in polyurethane. Polyurethane/CeO2 nanocomposite has high absorption at the region lower 350 nm.
The cationic polyurethane/CeO2 nanocomposite dispersion has been synthesized by adding ceria organosol to pre-polymer of polyurethane and then adding neutralization reagent and water to give an emulsion. FTIR analysis shows blue shift of the absorpsion band of CeO2. TEM micrograph shows that CeO2 nano-particles are uniformly dispersed in polyurethane. Polyurethane/CeO2 nanocomposite has high absorption at the region lower 350 nm.
2003, 20(3): 269-271
Abstract:
A kind of sulfobetaine, N,N-dimethyl-N-(3-sulfopropyl)-4-ethenyl-benzenemethanaminiuminner salt was synthesized from tertiary amine and propanesultone and characterized by IR and 1H NMR. The blood compatibilities of the polymers were evaluated by platelet adhesion method. No platelet adhesion in platelet rich plasma (PRP) was observed for two hours.
A kind of sulfobetaine, N,N-dimethyl-N-(3-sulfopropyl)-4-ethenyl-benzenemethanaminiuminner salt was synthesized from tertiary amine and propanesultone and characterized by IR and 1H NMR. The blood compatibilities of the polymers were evaluated by platelet adhesion method. No platelet adhesion in platelet rich plasma (PRP) was observed for two hours.
2003, 20(3): 272-274
Abstract:
Compound A was isolated from endophytic fungus (No.2526) of mangrove Avicennia from the South China Sea. The structure of compound A was elucidated by comprehensive spectral data and coincided with that of sterigmatocystin. Compound A showed a weak cytotoxic activity against Bel-7402 and NCIH-460 in vitro with IC50 96.53×10-6 and 72.52×10-6 g/mL respectively. It is the first report on sterigmatocystin that isolated from marine fungus.
Compound A was isolated from endophytic fungus (No.2526) of mangrove Avicennia from the South China Sea. The structure of compound A was elucidated by comprehensive spectral data and coincided with that of sterigmatocystin. Compound A showed a weak cytotoxic activity against Bel-7402 and NCIH-460 in vitro with IC50 96.53×10-6 and 72.52×10-6 g/mL respectively. It is the first report on sterigmatocystin that isolated from marine fungus.
2003, 20(3): 275-277
Abstract:
Iminodisuccinic acid is able to stabilize Cu2+ and Mn2+ in aqueous solutions of pH=7 and 11, with effect close to EDTA. It shows therefore a promising application in stabilization of H2O2 so lution used in pulp bleaching.
Iminodisuccinic acid is able to stabilize Cu2+ and Mn2+ in aqueous solutions of pH=7 and 11, with effect close to EDTA. It shows therefore a promising application in stabilization of H2O2 so lution used in pulp bleaching.
2003, 20(3): 278-280
Abstract:
An amphipathic Schiff base complex with Cu(Ⅱ) was synthesized from p-cresol and dodecanoyl chloride with total yield of 36.8%. The structure and amphipathic property of the ligand and Cu complex have been investigated. The oxidation of benzyl alcohol catalyzed by the complex in alkali solution gave benzaldehyde in yield of 57.8%.
An amphipathic Schiff base complex with Cu(Ⅱ) was synthesized from p-cresol and dodecanoyl chloride with total yield of 36.8%. The structure and amphipathic property of the ligand and Cu complex have been investigated. The oxidation of benzyl alcohol catalyzed by the complex in alkali solution gave benzaldehyde in yield of 57.8%.
2003, 20(3): 281-283
Abstract:
A facile synthesis of piperonol is reported from catechol. Reacted catechol with excess dichloromethane in an autoclave under nitrogen atmosphere gave 88.4% 1,3-benzodioxole (1), which is directly chloromethylated to yield 90.1% 5-chloromethyl 1,3-benzodioxole (2) by hydrogen chloride saturated triformol. 2 can easily convert to piperonal by treatment with alcoholic solution of Na2CO3 in yield of 97.7%. The total yield is 78%.
A facile synthesis of piperonol is reported from catechol. Reacted catechol with excess dichloromethane in an autoclave under nitrogen atmosphere gave 88.4% 1,3-benzodioxole (1), which is directly chloromethylated to yield 90.1% 5-chloromethyl 1,3-benzodioxole (2) by hydrogen chloride saturated triformol. 2 can easily convert to piperonal by treatment with alcoholic solution of Na2CO3 in yield of 97.7%. The total yield is 78%.
2003, 20(3): 284-286
Abstract:
The emulsion copolymerization of acrylates (methylmethacrylate,bulylacrylate acrylic acid,hydroxyethylmethacrylate) and vinyltriethoxysilane (VTS) using a reactive emulsifier DNS-86 has been studied as function of emulsifier amount, initiator amount, VTS amount, HEMA amount and polymerization temperature. The results showed that the monomer conversion increased with increase in emulsifier amount, initiator amount, amount of HEMA monomer and reaction temperature, but decreased with increase in the amount of VTS monomer.
The emulsion copolymerization of acrylates (methylmethacrylate,bulylacrylate acrylic acid,hydroxyethylmethacrylate) and vinyltriethoxysilane (VTS) using a reactive emulsifier DNS-86 has been studied as function of emulsifier amount, initiator amount, VTS amount, HEMA amount and polymerization temperature. The results showed that the monomer conversion increased with increase in emulsifier amount, initiator amount, amount of HEMA monomer and reaction temperature, but decreased with increase in the amount of VTS monomer.
2003, 20(3): 287-289
Abstract:
Six aromatic acid esters of heptaacetyl maltosyl were synthesized by reaction of hepta-O-acetyl-α-maltosyl bromide with corresponding aromatic acids, using triethyl benzyl ammonium chloride as a phase-transfer catalyst. In the 1H NMR spectra of these compounds, the chemical shift of C1-H in glycosyl-ring appears at downfield, the coupling constant J1-2=8.0~8.3. In the IR spectra of the products, the absorption of bending vibration of C1-H bond in glycosyl-ring appears at about 900 cm-1. The IR, 1H NMR spectra confirmed their β-anomer configuration. The greater relative abundances of the molecular ion peak were recorded in the mass spectra of the products. The method has advantages of mild reaction conditions, easy separation and high stereospecifi-city of the products.
Six aromatic acid esters of heptaacetyl maltosyl were synthesized by reaction of hepta-O-acetyl-α-maltosyl bromide with corresponding aromatic acids, using triethyl benzyl ammonium chloride as a phase-transfer catalyst. In the 1H NMR spectra of these compounds, the chemical shift of C1-H in glycosyl-ring appears at downfield, the coupling constant J1-2=8.0~8.3. In the IR spectra of the products, the absorption of bending vibration of C1-H bond in glycosyl-ring appears at about 900 cm-1. The IR, 1H NMR spectra confirmed their β-anomer configuration. The greater relative abundances of the molecular ion peak were recorded in the mass spectra of the products. The method has advantages of mild reaction conditions, easy separation and high stereospecifi-city of the products.
2003, 20(3): 290-292
Abstract:
A novel asymmetric dinuclear carboxylate-bridged Zn(Ⅱ) complex, [Zn2 (adam)4(phen)]·H2O (adam-=adamantanecarboxylato group, phen=1,10-phenanthroline), has been synthesized by reaction of adamantanecarbo xylic acid with Zn(CH3COO)2·2H2O in 1,10-phenanthroline. The crystal structure results as elucidated by XRD indicates that it is an adamantanecarboxylato Zn(Ⅱ) complex, in which the two Zn(Ⅱ) ions are triply-bridged by three adamantanecarboxylato groups, with a distance of 0.3259(1) nm between each other. In the dinuclear zinc complex, one Zn(Ⅱ) ion has a distorted tetrahedral geometry and the other has a distorted octahedral geometry.
A novel asymmetric dinuclear carboxylate-bridged Zn(Ⅱ) complex, [Zn2 (adam)4(phen)]·H2O (adam-=adamantanecarboxylato group, phen=1,10-phenanthroline), has been synthesized by reaction of adamantanecarbo xylic acid with Zn(CH3COO)2·2H2O in 1,10-phenanthroline. The crystal structure results as elucidated by XRD indicates that it is an adamantanecarboxylato Zn(Ⅱ) complex, in which the two Zn(Ⅱ) ions are triply-bridged by three adamantanecarboxylato groups, with a distance of 0.3259(1) nm between each other. In the dinuclear zinc complex, one Zn(Ⅱ) ion has a distorted tetrahedral geometry and the other has a distorted octahedral geometry.
2003, 20(3): 293-295
Abstract:
The behavior of poly (ethylene glycol)-b-poly(butylene terephthalate) copolymer has been investigated. The influences of the immersing time (in phosphate buffer solution of pH=7.4, at (37±1)℃) on the swelling ratio, the mass loss and the surface morphology of the copolymer film were examined. The copolymer is found to be degradable. The microspheres of PEG-b-PBT were prepared by a solvent extraction method using PVA as a stabilizer and characteristic of a smooth and spherical surface, sized about 1.133 μm. IR and XRD results reveal that Levonorgestrel crystalls are physically entrapped in the microspheres of the copolymer.
The behavior of poly (ethylene glycol)-b-poly(butylene terephthalate) copolymer has been investigated. The influences of the immersing time (in phosphate buffer solution of pH=7.4, at (37±1)℃) on the swelling ratio, the mass loss and the surface morphology of the copolymer film were examined. The copolymer is found to be degradable. The microspheres of PEG-b-PBT were prepared by a solvent extraction method using PVA as a stabilizer and characteristic of a smooth and spherical surface, sized about 1.133 μm. IR and XRD results reveal that Levonorgestrel crystalls are physically entrapped in the microspheres of the copolymer.
2003, 20(3): 296-298
Abstract:
Title compounds [Et3N-CH2Cl]+ [COO-Y-COOH]- (the latter is pyridine-2,6-dicarboxyl or dithio (bis-2,2'-benzoyloxy) were synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio (bis-2,2'-benzoic aicd) with CH2Cl2 and triethylamine in 1:1 molar ratio and characterized by elemental analysis, IR and 1H NMR. Their crystal structures were determined by X-ray single crystal diffractometry, the crystal (Ⅰ) belongs to orthorhombic with a=0.699043(14) nm, b=1.3489(3) nm, c=1.6689(3) nm, V=1.5745(6) nm3, Z=4, Dc=1.336 Mg/m3, μ=0.259 mm-1, R1=0.0334, wR2=0.0806, F(000)=672. The crystal (Ⅱ) belongs to triclinic with a=0.788(12) nm, b=1.239(19) nm, c=2.18(3) nm, α=89.2°, β=89.6°, γ=76.9°, V=2.078(55) nm3, Z=4, Dc=1.457 Mg/m3, μ=0.414 mm-1, R1=0.0620, wR2=0.1516, F(000)=960.
Title compounds [Et3N-CH2Cl]+ [COO-Y-COOH]- (the latter is pyridine-2,6-dicarboxyl or dithio (bis-2,2'-benzoyloxy) were synthesized by reaction of pyridine-2,6-dicarboxylic aicd or dithio (bis-2,2'-benzoic aicd) with CH2Cl2 and triethylamine in 1:1 molar ratio and characterized by elemental analysis, IR and 1H NMR. Their crystal structures were determined by X-ray single crystal diffractometry, the crystal (Ⅰ) belongs to orthorhombic with a=0.699043(14) nm, b=1.3489(3) nm, c=1.6689(3) nm, V=1.5745(6) nm3, Z=4, Dc=1.336 Mg/m3, μ=0.259 mm-1, R1=0.0334, wR2=0.0806, F(000)=672. The crystal (Ⅱ) belongs to triclinic with a=0.788(12) nm, b=1.239(19) nm, c=2.18(3) nm, α=89.2°, β=89.6°, γ=76.9°, V=2.078(55) nm3, Z=4, Dc=1.457 Mg/m3, μ=0.414 mm-1, R1=0.0620, wR2=0.1516, F(000)=960.
2003, 20(3): 299-301
Abstract:
Hydroxyapatite (HA) powders were prepared by hydrothermal treatment of CaHPO4·2H2O with Ca(OH)2 and characterized by XRD, FTIR, SEM, TEM. The results indicate that pH value and temperature show great influences on the structure and morphology of the products. At pH=9 and 120℃, the HA whis-kers were obtained with an aspect ratio>20, and typical diameter and length of 40 nm and 600 nm, respectively.
Hydroxyapatite (HA) powders were prepared by hydrothermal treatment of CaHPO4·2H2O with Ca(OH)2 and characterized by XRD, FTIR, SEM, TEM. The results indicate that pH value and temperature show great influences on the structure and morphology of the products. At pH=9 and 120℃, the HA whis-kers were obtained with an aspect ratio>20, and typical diameter and length of 40 nm and 600 nm, respectively.
2003, 20(3): 302-304
Abstract:
Ni(OH)2 nanoparticles were synthesized from reversed micelles consisted of AOT/iso-octane and Triton X-100/octanol/cyclohexane, respectively and characterized by UV-Vis, TEM and SEM, Ni(OH)2 wire was prepared from the system of AOT/iso-octane and Ni(OH)2 nano-powder was obtained in the system of Triton X-100/octanol/cyclohexane. The sizes of Ni(OH)2 powder, particle and wire were ~15 nm,~25 nm, and~60 nm, respectively.
Ni(OH)2 nanoparticles were synthesized from reversed micelles consisted of AOT/iso-octane and Triton X-100/octanol/cyclohexane, respectively and characterized by UV-Vis, TEM and SEM, Ni(OH)2 wire was prepared from the system of AOT/iso-octane and Ni(OH)2 nano-powder was obtained in the system of Triton X-100/octanol/cyclohexane. The sizes of Ni(OH)2 powder, particle and wire were ~15 nm,~25 nm, and~60 nm, respectively.
2003, 20(3): 305-306
Abstract:
At room temperature (25℃), urea and ferric chloride hexahydrate (system Ⅰ) or ferric nitrate nonahydrate (system Ⅱ) in a mole ratio of 6:1 were mixed and ground finely in an agate mortar for 6 hours, a direct solid state reaction occurred. IR and elemental analysis confirmed the products obtained are the com-plexes of urea with iron(Ⅲ).
At room temperature (25℃), urea and ferric chloride hexahydrate (system Ⅰ) or ferric nitrate nonahydrate (system Ⅱ) in a mole ratio of 6:1 were mixed and ground finely in an agate mortar for 6 hours, a direct solid state reaction occurred. IR and elemental analysis confirmed the products obtained are the com-plexes of urea with iron(Ⅲ).
