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2002 Volume 19 Issue 4
2002, 19(4): 307-309
Abstract:
Hemoglobin(Hb) is important as an oxygen carrier. The trace amount of oxygen in Hb was reduced by an electrolytic method using hydrogen as an electron donor. The deoxygenated Hb(deoxyHb) was stable against heat treatment at 60℃ with little precipitant. This method is safe, fast, and would be of potential use for large scale purification of Hb.
Hemoglobin(Hb) is important as an oxygen carrier. The trace amount of oxygen in Hb was reduced by an electrolytic method using hydrogen as an electron donor. The deoxygenated Hb(deoxyHb) was stable against heat treatment at 60℃ with little precipitant. This method is safe, fast, and would be of potential use for large scale purification of Hb.
2002, 19(4): 310-312
Abstract:
Some environmentally friendly catalysts such as HY and H-U zeolites, various cation-exchanged U zeolites, and some other solids have been used in the acylation reaction of ethylidenecyclohexane with acetic anhydride at room temperature to synthesize 3-(1-cyclohexenyl)-2-butanone instead of conventional catalysts. The effect of the amount of HY zeolite used on the acylation reaction was investigated. The yield of the acylated product was 72% in the case of n (ethylidenecyclohexane):n(acetic anhydride):m(HY zeolite)=1 mmol:10 mmol:0.100 g, reaction temperature:25℃, and reaction time:2 h. The regenerated HY zeolite showed almost the same catalytic activity as the fresh zeolite
Some environmentally friendly catalysts such as HY and H-U zeolites, various cation-exchanged U zeolites, and some other solids have been used in the acylation reaction of ethylidenecyclohexane with acetic anhydride at room temperature to synthesize 3-(1-cyclohexenyl)-2-butanone instead of conventional catalysts. The effect of the amount of HY zeolite used on the acylation reaction was investigated. The yield of the acylated product was 72% in the case of n (ethylidenecyclohexane):n(acetic anhydride):m(HY zeolite)=1 mmol:10 mmol:0.100 g, reaction temperature:25℃, and reaction time:2 h. The regenerated HY zeolite showed almost the same catalytic activity as the fresh zeolite
2002, 19(4): 313-316
Abstract:
Electrochemical impedance spectra of a nickel nanowire electrode at different applied potentials and their fitting results are given. The experimental results revealed that the electro chemical processes on the surface of the electrode were apparently influenced by the applied potentials. The electrochemical oxidation rate of Ni(Ⅱ) to Ni(Ⅲ) increased remarkably with the applied potential at a range of 0.10~0.40 V(vs.Ag/AgCl(1 mol/L KCl)). When the applied potential was higher than 0.4 V, the oxygen evolution reaction occurred simultaneously. The AC impedance measurements on a nickel bulk electrode and a nickel nanowire electrode under the same conditions showed the latter had much greater electrochemical activity and much faster reaction rate in the surface processes.
Electrochemical impedance spectra of a nickel nanowire electrode at different applied potentials and their fitting results are given. The experimental results revealed that the electro chemical processes on the surface of the electrode were apparently influenced by the applied potentials. The electrochemical oxidation rate of Ni(Ⅱ) to Ni(Ⅲ) increased remarkably with the applied potential at a range of 0.10~0.40 V(vs.Ag/AgCl(1 mol/L KCl)). When the applied potential was higher than 0.4 V, the oxygen evolution reaction occurred simultaneously. The AC impedance measurements on a nickel bulk electrode and a nickel nanowire electrode under the same conditions showed the latter had much greater electrochemical activity and much faster reaction rate in the surface processes.
2002, 19(4): 317-320
Abstract:
The adsorption behavior of organo bentonite to benzene/toluene/ethylbenzene/xylene(BTEX) and chromate in water was examined. The adsorption curves of organo bentonite for BTEX were well linear in range of 0 g/L to 0.2 g/L. The adsorption isotherm for chromate was agreed with Langmuir equation. The saturation adsorption capacity of organo bentonite to chromate was 571.21 mg/kg. Both adsorption quantities of organo bentonite to BTEX and chromate were found to be greatly increased in comparision with that of natural bentonite. The regeneration of chromate saturated organo bentonite was studied. The efficiency for extracting chromate from chromate saturated organo bentonite in alkaline solution was 84%.
The adsorption behavior of organo bentonite to benzene/toluene/ethylbenzene/xylene(BTEX) and chromate in water was examined. The adsorption curves of organo bentonite for BTEX were well linear in range of 0 g/L to 0.2 g/L. The adsorption isotherm for chromate was agreed with Langmuir equation. The saturation adsorption capacity of organo bentonite to chromate was 571.21 mg/kg. Both adsorption quantities of organo bentonite to BTEX and chromate were found to be greatly increased in comparision with that of natural bentonite. The regeneration of chromate saturated organo bentonite was studied. The efficiency for extracting chromate from chromate saturated organo bentonite in alkaline solution was 84%.
2002, 19(4): 321-324
Abstract:
An amphoteric polyurethane(APU) with both acid and base pendent groups was synthesized and a graft copolymer was obtained by reacting its NCO end group with OH and/or NH2 groups of the chitosan molecules in dilute HCl solution. The IR and DSC results indicated the occurence of hydrogen bonding in the copolymer. The graft copolymer in HCl solution appeared to be a dispersion with special rheological property.
An amphoteric polyurethane(APU) with both acid and base pendent groups was synthesized and a graft copolymer was obtained by reacting its NCO end group with OH and/or NH2 groups of the chitosan molecules in dilute HCl solution. The IR and DSC results indicated the occurence of hydrogen bonding in the copolymer. The graft copolymer in HCl solution appeared to be a dispersion with special rheological property.
2002, 19(4): 325-328
Abstract:
The O2·- scavenging activity of low molecular weight chitosan(LMC) and its complexes with Cu(Ⅱ), Co(Ⅱ), La(Ⅲ) was investigated. Colorimetric method was used, where VB2 and Met were used as producing reagent and NBT as detecting reagent for O2·-. The results showed that when mass concentration of samples was 0.5×10-2 g/mL, the O2·- scavenging activity of LMC-and LMC-Cu(Ⅱ), LMC-Co(Ⅱ), LMC-La(Ⅲ) were 80.3%, 98.9%, 84.1% and 78.4% respectively, but those of high molecular weight chitosan(820 kD) and D-Glucosamine were only about 13% and 9 5%. The scavenging activity of LMC and its complexes decreased with decrease in their mass concentration.
The O2·- scavenging activity of low molecular weight chitosan(LMC) and its complexes with Cu(Ⅱ), Co(Ⅱ), La(Ⅲ) was investigated. Colorimetric method was used, where V
2002, 19(4): 329-333
Abstract:
Cis-and trans dinitrodibenzo-14-crown-4 were synthesized via nitration of dibenzo-14-crown-4(DB14C4D) synthesized by a modified Pedersen method. Cis-and trans-diaminodibenzo-14-crown-4 (cis-DAmDB14C4 and trans-DAmDB14C4) were obtained by reduction of NO2 group using Pd/C catalyst. All the compounds were characterized by NMR, IR and elemental analysis. The stereo structures of the cis-and trans-diaminodibenzo-14-crown-4 in DMSO have been investigated by 1H NMR, 13C NMR and computer simulation.
Cis-and trans dinitrodibenzo-14-crown-4 were synthesized via nitration of dibenzo-14-crown-4(DB14C4D) synthesized by a modified Pedersen method. Cis-and trans-diaminodibenzo-14-crown-4 (cis-DAmDB14C4 and trans-DAmDB14C4) were obtained by reduction of NO2 group using Pd/C catalyst. All the compounds were characterized by NMR, IR and elemental analysis. The stereo structures of the cis-and trans-diaminodibenzo-14-crown-4 in DMSO have been investigated by 1H NMR, 13C NMR and computer simulation.
2002, 19(4): 334-337
Abstract:
Six complexes of N,N',N"-tri(3,5-dinitro benzenesulfonyl)-1,4,7-triazacyclononane(TDNBS-Tacn) with rare earth(La,Ce,Pr,Nd,Sm and Eu) were synthesized and their compositions were characterized by elemental analysis, 1H NMR, IR spectra and UV-Vis spectrum. Under the optimal conditions, the fluorescence spectra of complexes have a maximum excitation wavelength at 256 nm and maximum emission wavelength at 408 nm. The results indicate that the complexes have excellent luminescence properties.
Six complexes of N,N',N"-tri(3,5-dinitro benzenesulfonyl)-1,4,7-triazacyclononane(TDNBS-Tacn) with rare earth(La,Ce,Pr,Nd,Sm and Eu) were synthesized and their compositions were characterized by elemental analysis, 1H NMR, IR spectra and UV-Vis spectrum. Under the optimal conditions, the fluorescence spectra of complexes have a maximum excitation wavelength at 256 nm and maximum emission wavelength at 408 nm. The results indicate that the complexes have excellent luminescence properties.
2002, 19(4): 338-341
Abstract:
The influences of electrolytes(NaCl、MgCl2 and AlCl3) and partially hydrolyzed polyacrylamide (PHPA) on the thixotropy of magnesium aluminum mixed metal hydroxide(Mg-Al-MMH) kaolinite suspension have been studied. The results show that the thixotropic fluid type of Mg-Al-MMH kaolinite suspension with mass ratio of MMH to kaolinite R=0.029 was independent of the concentration of the electrolytes, whereas increase in electrolyte concentration could cause Mg-Al-MMH kaolinite system with R=0.129 to be transformed from complex thixotropy to positive thixotropy. With the increase of PHPA content, the thixotropic type of the MMH kaolinite suspension with R=0.029 transformed from positive thixotropy to complex thixotropy and the suspension with R=0.129 from complex to negative thixotropy. All the three electropytes and PHPA could reduce the viscosity of the Mg-Al-MMH kaolinite suspensions. The mechanism of the thixotropy has been discussed briefly.
The influences of electrolytes(NaCl、MgCl2 and AlCl3) and partially hydrolyzed polyacrylamide (PHPA) on the thixotropy of magnesium aluminum mixed metal hydroxide(Mg-Al-MMH) kaolinite suspension have been studied. The results show that the thixotropic fluid type of Mg-Al-MMH kaolinite suspension with mass ratio of MMH to kaolinite R=0.029 was independent of the concentration of the electrolytes, whereas increase in electrolyte concentration could cause Mg-Al-MMH kaolinite system with R=0.129 to be transformed from complex thixotropy to positive thixotropy. With the increase of PHPA content, the thixotropic type of the MMH kaolinite suspension with R=0.029 transformed from positive thixotropy to complex thixotropy and the suspension with R=0.129 from complex to negative thixotropy. All the three electropytes and PHPA could reduce the viscosity of the Mg-Al-MMH kaolinite suspensions. The mechanism of the thixotropy has been discussed briefly.
2002, 19(4): 342-345
Abstract:
Five heteropoly compound(HPC) isomers T-K6[SiW11TiO40]·xH2O and T-,Ui-K6[SiW11TiO40]·xH2O(Ui=U1,U2,U3) were synthesized and characterized. The IR, UV spectrometry, polarography and chemical titration results confirmed the existence of TiO2 groups in the complexes. The 183W NMR spectra of all of the complexes revealed the Keggin structure of anions in the compounds. The experiment of catalytic oxidation of maleic acid by H2O2 showed the catalytic activities of these complexes were higher than those of their corresponding complexes without peoxo ions, and catalytic activies of U-isomer was higher than T-isomer.
Five heteropoly compound(HPC) isomers T-K6[SiW11TiO40]·xH2O and T-,Ui-K6[SiW11TiO40]·xH2O(Ui=U1,U2,U3) were synthesized and characterized. The IR, UV spectrometry, polarography and chemical titration results confirmed the existence of TiO2 groups in the complexes. The 183W NMR spectra of all of the complexes revealed the Keggin structure of anions in the compounds. The experiment of catalytic oxidation of maleic acid by H2O2 showed the catalytic activities of these complexes were higher than those of their corresponding complexes without peoxo ions, and catalytic activies of U-isomer was higher than T-isomer.
2002, 19(4): 346-350
Abstract:
Ullmann reaction of p-chlorophenol(X) with 2,4-dichloroacetophenone(Ⅺ) was studied as functions of catalysts, solvent, reactants ratio and microwave irradiation. The reaction products were characterized by GC-MS, 1H NMR and IR techniques. It is found that some catalysts have good regio selectivity for Ullmann reaction. With Cu2Cl2 as catalyst, AcNMe 2/Xylene as mixed solvent high yield of target compound was obtained. Microwave irradiation was found to accelerate the reaction.
Ullmann reaction of p-chlorophenol(X) with 2,4-dichloroacetophenone(Ⅺ) was studied as functions of catalysts, solvent, reactants ratio and microwave irradiation. The reaction products were characterized by GC-MS, 1H NMR and IR techniques. It is found that some catalysts have good regio selectivity for Ullmann reaction. With Cu2Cl2 as catalyst, AcNMe 2/Xylene as mixed solvent high yield of target compound was obtained. Microwave irradiation was found to accelerate the reaction.
2002, 19(4): 351-354
Abstract:
2-Hydroxypropyltrimethyl ammonium chloride chitosan(HACC), a water solube quaternary ammonium salt of chitosan, was prepared by the reaction of chitosan with 2,3-epoxypropyltrimethyl ammonium chloride. The content of quaternary cations(R4N+) determined by the method of colloid titration with polyanion(PVSK) was 3.39 mmol/g, the content and degree of substitution of R4N+ in N atom were 3.07 mmol/g and 58.1% respectively. IR spectra revealed that the most substituents were attached on N atom of chitosan. The moisture adsorbability of HACC was as good as that of hyaluronic acid(HA), the moisture retentivity of HACC was better than that of HA, the minimum inhibitory concentration(MIC) of HACC for staptytococous aureus(ATCC25293) was 625 mg/L.
2-Hydroxypropyltrimethyl ammonium chloride chitosan(HACC), a water solube quaternary ammonium salt of chitosan, was prepared by the reaction of chitosan with 2,3-epoxypropyltrimethyl ammonium chloride. The content of quaternary cations(R4N+) determined by the method of colloid titration with polyanion(PVSK) was 3.39 mmol/g, the content and degree of substitution of R4N+ in N atom were 3.07 mmol/g and 58.1% respectively. IR spectra revealed that the most substituents were attached on N atom of chitosan. The moisture adsorbability of HACC was as good as that of hyaluronic acid(HA), the moisture retentivity of HACC was better than that of HA, the minimum inhibitory concentration(MIC) of HACC for staptytococous aureus(ATCC25293) was 625 mg/L.
2002, 19(4): 355-358
Abstract:
The effects of cations, anions and organic substances on the structure and property of oxidation films of Al alloy have been investigated. The results showed that the thickness and hardness of the oxidation films can be increased by adding the additives at 35℃. The mixture or complex of the above substances can be as complicated additives for oxidation film of Al alloy at medium temperature. The structure of oxidation film formed at 35℃ with complicated additives was fine and close in texture. The property of oxidation film of Al alloy in the solution with organic substance additives is the best and that with cation additives is the worst.
The effects of cations, anions and organic substances on the structure and property of oxidation films of Al alloy have been investigated. The results showed that the thickness and hardness of the oxidation films can be increased by adding the additives at 35℃. The mixture or complex of the above substances can be as complicated additives for oxidation film of Al alloy at medium temperature. The structure of oxidation film formed at 35℃ with complicated additives was fine and close in texture. The property of oxidation film of Al alloy in the solution with organic substance additives is the best and that with cation additives is the worst.
2002, 19(4): 359-363
Abstract:
A novel amphiphilic phosphine ligand N,N-bis(diphenylphosphinomethyl)piperazine was synthesized by reaction of piperazine with[Ph2P(CH2OH)2]+Cl- in the medium with pH ranged in 9~10 at 65~70℃ for 2.5 h in 97% yield, and characterized by elemental analysis, NMR, MS, IR and UV. Its palladium complexes with different molar ratio of Ph2P to Pd were prepared in n-butanol. XPS data revealed that the coordination bonds were formed between phosphorous and palladium atoms in the palladium complexes 1a, 1b. High catalytic activities of the complexes 1a, 1b were observed in carbonylation of benzyl chloride with CO. The catalyst could be reused repeatedly in five times.
A novel amphiphilic phosphine ligand N,N-bis(diphenylphosphinomethyl)piperazine was synthesized by reaction of piperazine with[Ph2P(CH2OH)2]
2002, 19(4): 364-368
Abstract:
4-Alkyl-cyclohexanecarboxylic acids as liquid crystal intermediates were synthesized from hydrogenation of 4-alkylbenzoic acids over Raney Ni. The relation of the alkyl group with the conformational isomer has been investigated. It is found that the longer the length of the alkyl group, the slower the conversion of the acid in NaOH solution. The hydrogen pressure of 7.1 MPa was found to be enough for hydrogenation in a mixed solvent of THF and cyclohexane. The trans/cis isomer ratio of the products was more than 2, and the transformation free energy of the conformational isomer increased with the increase of the carbon atom numbers of the alkyl group.
4-Alkyl-cyclohexanecarboxylic acids as liquid crystal intermediates were synthesized from hydrogenation of 4-alkylbenzoic acids over Raney Ni. The relation of the alkyl group with the conformational isomer has been investigated. It is found that the longer the length of the alkyl group, the slower the conversion of the acid in NaOH solution. The hydrogen pressure of 7.1 MPa was found to be enough for hydrogenation in a mixed solvent of THF and cyclohexane. The trans/cis isomer ratio of the products was more than 2, and the transformation free energy of the conformational isomer increased with the increase of the carbon atom numbers of the alkyl group.
2002, 19(4): 369-372
Abstract:
A variety of nickel electrodes containing Zn were prepared by doping and by coprecipitation. The effects of Zn addition methods on the electric properties of the nickel electrode were studied. The results show that addition of Zn either by doping or by coprecipitation can improve the electric properties of nickel electrode, the charge efficiency and the transportation ability of H+, whereas the later method appeared better. The cyclic voltammetry revealed an improvement of the reversibility of nickel electrode. The optimum Zn content was 1.0%~3.0%.
A variety of nickel electrodes containing Zn were prepared by doping and by coprecipitation. The effects of Zn addition methods on the electric properties of the nickel electrode were studied. The results show that addition of Zn either by doping or by coprecipitation can improve the electric properties of nickel electrode, the charge efficiency and the transportation ability of H+, whereas the later method appeared better. The cyclic voltammetry revealed an improvement of the reversibility of nickel electrode. The optimum Zn content was 1.0%~3.0%.
2002, 19(4): 373-376
Abstract:
The structures and compositions of castor oil and its ethoxylate derivative have been characterized by means of NMR and IR spectroscopy and MS spectrometry. The spectral band assignments are confirmed by Gradient Correlated Spectroscopy(gCOSY), Gradient 1H-detected Heteronuclear Single-Quantum Coherence(gHSQC), Gradient 1H-detected Heteronuclear Multiple-Bond Correlation(gHMBC) and Distortionless Enhancement by Polarization Transfer(DEPT) techniques. The results show that there are at least six series compounds in ethoxylate derivative of castor oil.
The structures and compositions of castor oil and its ethoxylate derivative have been characterized by means of NMR and IR spectroscopy and MS spectrometry. The spectral band assignments are confirmed by Gradient Correlated Spectroscopy(gCOSY), Gradient 1H-detected Heteronuclear Single-Quantum Coherence(gHSQC), Gradient 1H-detected Heteronuclear Multiple-Bond Correlation(gHMBC) and Distortionless Enhancement by Polarization Transfer(DEPT) techniques. The results show that there are at least six series compounds in ethoxylate derivative of castor oil.
2002, 19(4): 377-380
Abstract:
A series of SO42-/ZrO2 TiO2 solid superacids(SZT) were prepared from a solution of ZnOCl2·8H2O and TiCl4, using ammonia water as a precipitant with or without addition of lanthanum nitrate, followed by aging at different temperature and calcining at 550℃ or 600℃. The acid strengths of SZT were evaluated by a flowing indicator method. The IR and XRD results showed that the superacid with molar ratio of Zr to Ti=0.5, aged at -15℃ and calcined at 550℃ with addition of La(NO3)3 has an anatase structure and more superacid active sites. Yield of 97.1% was achieved in catalytic esterification of acetic acid with n-butanol by using this catalyst.
A series of SO42-/ZrO2 TiO2 solid superacids(SZT) were prepared from a solution of ZnOCl2·8H2O and TiCl4, using ammonia water as a precipitant with or without addition of lanthanum nitrate, followed by aging at different temperature and calcining at 550℃ or 600℃. The acid strengths of SZT were evaluated by a flowing indicator method. The IR and XRD results showed that the superacid with molar ratio of Zr to Ti=0.5, aged at -15℃ and calcined at 550℃ with addition of La(NO3)3 has an anatase structure and more superacid active sites. Yield of 97.1% was achieved in catalytic esterification of acetic acid with n-butanol by using this catalyst.
2002, 19(4): 381-383
Abstract:
1-(Pyridylazo)-2-naphthol(PAN) can cause a sensitive incision on the oscillogram in NaOH solution, and the incision depth would decrease linearly with the increase of the concentration of Co2+. Based on this oscillographic characteristic, second order differential oscillographic voltammety is developed for Co2+ determination. The linear range of the determination of Co2+ is 2.00×10-7~8.20×10-6 mol/L and the detection limit is 1.00×10-7 mol/L. RSD is 1.8% for eight successful determinations of 4.20×10-6 mol/L Co2+. Satisfactory results were obtained by this method in determination of VB12 content in VB12 injection liquid.
1-(Pyridylazo)-2-naphthol(PAN) can cause a sensitive incision on the oscillogram in NaOH solution, and the incision depth would decrease linearly with the increase of the concentration of Co2+. Based on this oscillographic characteristic, second order differential oscillographic voltammety is developed for Co2+ determination. The linear range of the determination of Co2+ is 2.00×10-7~8.20×10-6 mol/L and the detection limit is 1.00×10-7 mol/L. RSD is 1.8% for eight successful determinations of 4.20×10-6 mol/L Co2+. Satisfactory results were obtained by this method in determination of VB12 content in VB12 injection liquid.
2002, 19(4): 384-386
Abstract:
Six secondary metabolites 1~6 were separated from the soft coral Sinularia sp. collected from Sanya bay in Hainan province China. Their structures were identified by spectroscopic methods to be 24-methylene-cholest-4-en-3U,6U-diol(1), 24-methylene cholest-4-en-3U,7T-diol(2), gorgosterol(3), cholesterol(4), batyl alcohol(5) and thymine(6).
Six secondary metabolites 1~6 were separated from the soft coral Sinularia sp. collected from Sanya bay in Hainan province China. Their structures were identified by spectroscopic methods to be 24-methylene-cholest-4-en-3U,6U-diol(1), 24-methylene cholest-4-en-3U,7T-diol(2), gorgosterol(3), cholesterol(4), batyl alcohol(5) and thymine(6).
2002, 19(4): 387-389
Abstract:
Three thyroxine haptens were synthesized by protecting amino group of thyroxine with Cu 2+ ion and characterized by 1H NMR, MS, elemental analysis and IR. Thyroxine and the derivatives were coupled with carrier proteins(BSA and Ovalbumin). Thus antigens were prepared and hapten quantities of the antigens were measured by UV spectroscopy at 320 nm. An anti-O-methyl-T4 monoclonal antibody was prepared by immunization, cell fusion and screening.
Three thyroxine haptens were synthesized by protecting amino group of thyroxine with Cu 2+ ion and characterized by 1H NMR, MS, elemental analysis and IR. Thyroxine and the derivatives were coupled with carrier proteins(BSA and Ovalbumin). Thus antigens were prepared and hapten quantities of the antigens were measured by UV spectroscopy at 320 nm. An anti-O-methyl-T4 monoclonal antibody was prepared by immunization, cell fusion and screening.
SERS Studies of Corrosion Inhibition of BTA and Its Derivative on Copper Electrodes in NaCl Solution
2002, 19(4): 390-392
Abstract:
Corrosion inhibition of benzotriazole(BTA) and its derivative CBTME on Cu in 3%NaCl solution was studied by SERS technique. The inhibition mechanism for BTA and CBTME on copper corrosion in the solution was found to be similar each other, by which a protective film is formed through the triazole ring. The substituent group (-COOCH3) of CBTME plays the role in the inhibition effect due to steric hindrance. A combination of BTA and CBTME showed a synergistic effect and the inhibition mechanism remained the same as individual species.
Corrosion inhibition of benzotriazole(BTA) and its derivative CBTME on Cu in 3%NaCl solution was studied by SERS technique. The inhibition mechanism for BTA and CBTME on copper corrosion in the solution was found to be similar each other, by which a protective film is formed through the triazole ring. The substituent group (-COOCH3) of CBTME plays the role in the inhibition effect due to steric hindrance. A combination of BTA and CBTME showed a synergistic effect and the inhibition mechanism remained the same as individual species.
2002, 19(4): 393-395
Abstract:
Twentyone N,N'-nitrobenzoyl substituted benzoylthiosemicarbazides were synthesized by addition reaction of nitrophenyl isothiocyanates with aroyl hydrazines and their structures were characterized by 1H NMR, 13C NMR, IR and elemental analysis. The biological tests indicated that these compounds had antibacterial activity against B.subtilis, but no action on E.coli.
Twentyone N,N'-nitrobenzoyl substituted benzoylthiosemicarbazides were synthesized by addition reaction of nitrophenyl isothiocyanates with aroyl hydrazines and their structures were characterized by 1H NMR, 13C NMR, IR and elemental analysis. The biological tests indicated that these compounds had antibacterial activity against B.subtilis, but no action on E.coli.
2002, 19(4): 396-397
Abstract:
The-3-(4-aminophenylazo)benzenesulfonic sodium and 3-(4-amino-3-methylphenylazo) benzenesulfonic sodium have been synthesized via protecting NH2 group in aniline o-toluidine by -CH2SO3Na and characterized by IR and 13C NMR.
The-3-(4-aminophenylazo)benzenesulfonic sodium and 3-(4-amino-3-methylphenylazo) benzenesulfonic sodium have been synthesized via protecting NH2 group in aniline o-toluidine by -CH2SO3Na and characterized by IR and 13C NMR.
2002, 19(4): 398-400
Abstract:
Potentiometric titration method was used to judge whether the precipitated hydroxide is a complex hydroxide or a mixture when alkali solution was added to an aqueous solution containing two kinds of metal salts(Al3+、Fe3+、Ni2+、Zn 2+、Cu2+). Capability of complex formation between the metal hydroxides was investigated by comparing the pH of the plateau in the titration curves with that for the solution of one metal ion. Complex hydroxide was formed for all divalent ions and trivalent ions, and the sequence of the capability was Ni2+ > Zn2+ > Cu2+.
Potentiometric titration method was used to judge whether the precipitated hydroxide is a complex hydroxide or a mixture when alkali solution was added to an aqueous solution containing two kinds of metal salts(Al3+、Fe3+、Ni2+、Zn 2+、Cu2+). Capability of complex formation between the metal hydroxides was investigated by comparing the pH of the plateau in the titration curves with that for the solution of one metal ion. Complex hydroxide was formed for all divalent ions and trivalent ions, and the sequence of the capability was Ni2+ > Zn2+ > Cu2+.
2002, 19(4): 401-403
Abstract:
A series of 2-amimo-3-cyano-7,7-dimethyl-4-aryl-5-oxo-5,6,7,8-tetra-4H-chromenes were synthesized in the absence of catalyst. Their structures were determined by IR, 1H NMR, and single crystal X-ray diffraction.
A series of 2-amimo-3-cyano-7,7-dimethyl-4-aryl-5-oxo-5,6,7,8-tetra-4H-chromenes were synthesized in the absence of catalyst. Their structures were determined by IR, 1H NMR, and single crystal X-ray diffraction.
2002, 19(4): 404-406
Abstract:
Alkylation of diethyl 3-oxoglutarate monoanion by 4-bromobutene to produce enone diester 3, subsequent alkylation of 3 with 4-bromo-1-butene using K2CO3 and a catalytic amount of NaIin the mixed solvent afforded dienone diester 4, which underwent decarboxylative hydrolysis when treated with 15% KOH in methanol under refluxing to provide dienone 5. The dienone afforded 2,8-dimethyl-1,7-dioxaspiroundecane 1 in good yield and high purity via an oxymercuration-cyclisation-reduction sequence.
Alkylation of diethyl 3-oxoglutarate monoanion by 4-bromobutene to produce enone diester 3, subsequent alkylation of 3 with 4-bromo-1-butene using K2CO3 and a catalytic amount of NaIin the mixed solvent afforded dienone diester 4, which underwent decarboxylative hydrolysis when treated with 15% KOH in methanol under refluxing to provide dienone 5. The dienone afforded 2,8-dimethyl-1,7-dioxaspiroundecane 1 in good yield and high purity via an oxymercuration-cyclisation-reduction sequence.
2002, 19(4): 407-408
Abstract:
Ammonium thiocyanate was prepared in 2 steps from aqueous ammonia and carbon disulfied by phase transfer catalysis in yield of 72.7%, when catalysts consisted of OP-4 and OP-21 in mole ratio of 4:6. The effects of reaction temperature, time, mole ratio of OP-4 to OP-21 and conparison with other catalysts on the reaction were descurved.
Ammonium thiocyanate was prepared in 2 steps from aqueous ammonia and carbon disulfied by phase transfer catalysis in yield of 72.7%, when catalysts consisted of OP-4 and OP-21 in mole ratio of 4:6. The effects of reaction temperature, time, mole ratio of OP-4 to OP-21 and conparison with other catalysts on the reaction were descurved.
