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2018 Volume 81 Issue 5
2018, 81(5): 387-393
Abstract:
As a kind of metal-free sp2 conjugated polymer semiconductor, g-C3N4 nanosheets have a wide range of application in the fields of photoelectrochemistry, catalysis, photocatalysis, biomedicine and so on. This paper reviews the recent study on the preparation of two-dimensional g-C3N4 nanosheets. The advantages and disadvantages of different methods for preparation of g-C3N4 nanosheets are summarized. Finally, the prospects for future investigations of two-dimensional g-C3N4 nanosheets are proposed.
As a kind of metal-free sp2 conjugated polymer semiconductor, g-C3N4 nanosheets have a wide range of application in the fields of photoelectrochemistry, catalysis, photocatalysis, biomedicine and so on. This paper reviews the recent study on the preparation of two-dimensional g-C3N4 nanosheets. The advantages and disadvantages of different methods for preparation of g-C3N4 nanosheets are summarized. Finally, the prospects for future investigations of two-dimensional g-C3N4 nanosheets are proposed.
2018, 81(5): 394-401
Abstract:
As a kind of unique sorbent for selectively separating and enriching cis-diol-containing biomolecules, boronate affinity materials have gained more and more attention in the last decade. Meanwhile, a variety of new materials with boronate affinity function are being developed and widely used in affinity separation, disease diagnostics, aptamer selection, drug delivery and biosensor. Finally, the development trends of boronate affinity materials are proposed.
As a kind of unique sorbent for selectively separating and enriching cis-diol-containing biomolecules, boronate affinity materials have gained more and more attention in the last decade. Meanwhile, a variety of new materials with boronate affinity function are being developed and widely used in affinity separation, disease diagnostics, aptamer selection, drug delivery and biosensor. Finally, the development trends of boronate affinity materials are proposed.
2018, 81(5): 402-408
Abstract:
Efficient, green and low-energy CO2 capture technology is the key to solving the problem of energy gas purification and greenhouse gas emission reduction. Membrane separation technology has potential prospects for development because of its high efficiency, energy saving, low carbon and other characteristics in the field of CO2 capture. At present, the study of CO2 separation membrane mainly focuses on the filler in mixed matrix membrane (MMMs), and the "trade-off" effect between membrane permeability and selectivity is controlled by adjusting the filler. MMMs separation technology show a good application prospects in the field of gas separation. In recent years, researchers have found that the filler is usually a key factor affecting separation performance of the MMMs, and the use of different fillers can improve the gas separation performance of the mixed matrix membrane. This paper summarizes the filler that has been developed at present, so as to provide a reference for the design and development of new MMMs for CO2 separation.
Efficient, green and low-energy CO2 capture technology is the key to solving the problem of energy gas purification and greenhouse gas emission reduction. Membrane separation technology has potential prospects for development because of its high efficiency, energy saving, low carbon and other characteristics in the field of CO2 capture. At present, the study of CO2 separation membrane mainly focuses on the filler in mixed matrix membrane (MMMs), and the "trade-off" effect between membrane permeability and selectivity is controlled by adjusting the filler. MMMs separation technology show a good application prospects in the field of gas separation. In recent years, researchers have found that the filler is usually a key factor affecting separation performance of the MMMs, and the use of different fillers can improve the gas separation performance of the mixed matrix membrane. This paper summarizes the filler that has been developed at present, so as to provide a reference for the design and development of new MMMs for CO2 separation.
2018, 81(5): 409-413
Abstract:
The nitrogen-activated C=C double bonds of enamides have considerable potential for use in the construction of various nitrogen-containing products, and organocatalyzed α, β-difunctionalization of nitrogen-activated double bonds proved to be an efficient and versatile concept, and allowed us to obtain a wide range of useful building blocks. The Povarov reaction with enamides, an extended method for vicinal difunctionalization, provides a straightforward and modular entry to 4-amino-1, 2, 3, 4-tetrahydroquinolines. Despite its importance, it was only very recently that several highly efficient catalytic asymmetric protocols for this reaction have been developed as summarized in this review.
The nitrogen-activated C=C double bonds of enamides have considerable potential for use in the construction of various nitrogen-containing products, and organocatalyzed α, β-difunctionalization of nitrogen-activated double bonds proved to be an efficient and versatile concept, and allowed us to obtain a wide range of useful building blocks. The Povarov reaction with enamides, an extended method for vicinal difunctionalization, provides a straightforward and modular entry to 4-amino-1, 2, 3, 4-tetrahydroquinolines. Despite its importance, it was only very recently that several highly efficient catalytic asymmetric protocols for this reaction have been developed as summarized in this review.
2018, 81(5): 414-424
Abstract:
Moxifloxacin is a fourth-generation quinolone antibiotic, which has broad antibacterial spectrum, strong effect, low toxicity, so it is widely used in clinics. Moxifloxacin impurities were produced during process of synthesis and storage, the impurities must be controlled respectively to ensure the security and effect of the moxifloxacin drug. In this paper, the recent development in synthesis of moxifloxacin and its impurities was reviewed.
Moxifloxacin is a fourth-generation quinolone antibiotic, which has broad antibacterial spectrum, strong effect, low toxicity, so it is widely used in clinics. Moxifloxacin impurities were produced during process of synthesis and storage, the impurities must be controlled respectively to ensure the security and effect of the moxifloxacin drug. In this paper, the recent development in synthesis of moxifloxacin and its impurities was reviewed.
2018, 81(5): 425-432
Abstract:
Efficient conversion of cellulose catalyzed by cheap transition metal instead of strong acid and noble metal catalysts is the development direction of green chemical industry, which has been the focus of many researchers. In this paper, the applications of transition metal-based catalysts in cellulose conversion are reviewed from cellulose pyrolysis (including liquefation and gasification), cellulose hydrolysis, hydrogenolysis and cellulose degradation into 5-hydroxymethyl furfural (5-HMF) respectively, and the type of catalysts, reaction conditions and reaction mechanism are summarized. Finally, the problems in the transition metal catalysis process are pointed out, and the research direction is prospected.
Efficient conversion of cellulose catalyzed by cheap transition metal instead of strong acid and noble metal catalysts is the development direction of green chemical industry, which has been the focus of many researchers. In this paper, the applications of transition metal-based catalysts in cellulose conversion are reviewed from cellulose pyrolysis (including liquefation and gasification), cellulose hydrolysis, hydrogenolysis and cellulose degradation into 5-hydroxymethyl furfural (5-HMF) respectively, and the type of catalysts, reaction conditions and reaction mechanism are summarized. Finally, the problems in the transition metal catalysis process are pointed out, and the research direction is prospected.
2018, 81(5): 433-438
Abstract:
Using homemade biomass activated carbon (BAC) as raw material, TiO2/bio-activated carbon (TiO2/BAC) were synthesized by sol-gel method. The TiO2/BAC was characterized by SEM, FTIR, XRD and nitrogen adsorption isotherms. The adsorption performance of the composite materials on neutral red, methylene blue and formaldehyde was studied. The results showed that, when the addition of biomass activated carbon was 7g in preparing of the composite material, i.e.BAC(wt)/(BuO)4Ti (vol)=1:5, the amount of composite material was 0.7g and the pre-adsorption time was 2 h, the composite material has the best adsorption degradation effect for dyes. The adsorption degradation rate of the TiO2/BAC composites material still reached more than 80% after 5 cycles of reuse. When the addition of biomass activated carbon was 6 g and the addition of composites material was 2 g, the adsorption degradation rate of the composite material to formaldehyde reached a maximum of 63.41%. The composite material is expected to be used for the removal of methylene blue and neutral red in wastewater and the degradation of formaldehyde in indoor environment.
Using homemade biomass activated carbon (BAC) as raw material, TiO2/bio-activated carbon (TiO2/BAC) were synthesized by sol-gel method. The TiO2/BAC was characterized by SEM, FTIR, XRD and nitrogen adsorption isotherms. The adsorption performance of the composite materials on neutral red, methylene blue and formaldehyde was studied. The results showed that, when the addition of biomass activated carbon was 7g in preparing of the composite material, i.e.BAC(wt)/(BuO)4Ti (vol)=1:5, the amount of composite material was 0.7g and the pre-adsorption time was 2 h, the composite material has the best adsorption degradation effect for dyes. The adsorption degradation rate of the TiO2/BAC composites material still reached more than 80% after 5 cycles of reuse. When the addition of biomass activated carbon was 6 g and the addition of composites material was 2 g, the adsorption degradation rate of the composite material to formaldehyde reached a maximum of 63.41%. The composite material is expected to be used for the removal of methylene blue and neutral red in wastewater and the degradation of formaldehyde in indoor environment.
2018, 81(5): 439-444
Abstract:
With special tetrahedral layer in the structure, "114" compounds have potential application value in terms of magnetics and oxygen storage. In this article, conventional high-temperature solid-state reaction method is used to synthesize new compound YBaZn3GaO7, in which Sc3+ with smaller effective radius is doped in octahedral site to obtain the total solid solution compound Y1-xScxBaZn3GaO7(x=0~1). Structural refining determines the space group of the series of "114" compounds to be P63mc, and structural analysis shows that the structure has obvious evolution trend with increasing doping amount. From YBaZn3GaO7 to ScBaZn3GaO, the cell parameter decreases linearly. In addition, according to analysis on bond length of each coordination element, increasing doping quantity may reduce structural aberration and stress to allow for integration of Zn2+ and Ga3+ in tetrahedral coordination, thus obtaining "114" compounds with more stable structure.
With special tetrahedral layer in the structure, "114" compounds have potential application value in terms of magnetics and oxygen storage. In this article, conventional high-temperature solid-state reaction method is used to synthesize new compound YBaZn3GaO7, in which Sc3+ with smaller effective radius is doped in octahedral site to obtain the total solid solution compound Y1-xScxBaZn3GaO7(x=0~1). Structural refining determines the space group of the series of "114" compounds to be P63mc, and structural analysis shows that the structure has obvious evolution trend with increasing doping amount. From YBaZn3GaO7 to ScBaZn3GaO, the cell parameter decreases linearly. In addition, according to analysis on bond length of each coordination element, increasing doping quantity may reduce structural aberration and stress to allow for integration of Zn2+ and Ga3+ in tetrahedral coordination, thus obtaining "114" compounds with more stable structure.
2018, 81(5): 445-449
Abstract:
Mass Spectrometry online monitoring of organic chemical reaction can capture the signal and change of the reactants, intermediates, and products in the reaction process in real time so as to deepen the understanding of the nature of the reaction. In this study, extractive electrospray ionization tandem mass spectrometry (EESI-MS) were used to monitor Friedlander condensation reaction of 2-aminoacetophenone and acetylacetone using oxalate as a catalyst. At different time of the reaction, the molecular ion peak of reactants (m/z 136), intermediates (m/z 236, m/z 218) and product (m/z 200) signal were captured, the changes of them in the course of the reaction with time trends were recorded, the reaction mechanism was deduced.
Mass Spectrometry online monitoring of organic chemical reaction can capture the signal and change of the reactants, intermediates, and products in the reaction process in real time so as to deepen the understanding of the nature of the reaction. In this study, extractive electrospray ionization tandem mass spectrometry (EESI-MS) were used to monitor Friedlander condensation reaction of 2-aminoacetophenone and acetylacetone using oxalate as a catalyst. At different time of the reaction, the molecular ion peak of reactants (m/z 136), intermediates (m/z 236, m/z 218) and product (m/z 200) signal were captured, the changes of them in the course of the reaction with time trends were recorded, the reaction mechanism was deduced.
2018, 81(5): 450-455
Abstract:
A novel fluorescent sensor (HF-1) for iron ion bearing coumarin-benzimidazole derivatives have been designed and synthesized. The structure of the sensor was characterized by IR, 1H NMR and MS. Nitrogen and oxygen heteroatoms as chelating sites and ethyl-7-hydroxycoumarin-3-carboxylate group was introduced as fluorophore to achieve recognitions. HF-1 displays high selectivity and sensitivity for iron ion in a very short time, which serves as an on-off type sensor. In addition, the probe HF-1 has the advantages of simple synthesis route, low cost and high yield. The sensor has potential applications in physiological and environmental systems for iron ion detection.
A novel fluorescent sensor (HF-1) for iron ion bearing coumarin-benzimidazole derivatives have been designed and synthesized. The structure of the sensor was characterized by IR, 1H NMR and MS. Nitrogen and oxygen heteroatoms as chelating sites and ethyl-7-hydroxycoumarin-3-carboxylate group was introduced as fluorophore to achieve recognitions. HF-1 displays high selectivity and sensitivity for iron ion in a very short time, which serves as an on-off type sensor. In addition, the probe HF-1 has the advantages of simple synthesis route, low cost and high yield. The sensor has potential applications in physiological and environmental systems for iron ion detection.
2018, 81(5): 456-460
Abstract:
Study on new anticancer drugs is one of the key tasks of global drug development. We previously found that 3, 5-disubstituted-1H-indole derivatives have apparent inhibitory activity against pancreatic cancer cells. Here we reported a new simple and efficient route for the synthesis of 3-((substituted-thio)methyl)-5-acylamino-1H-indole derivatives, which involves Vilsmeier-Haack reaction, Boc protection of secondary amine, aldehyde reduction, carboxylic acid and amine condensation reaction, and eight new target compounds (11a~11h) were synthesized. The cell-based assays revealed that 11a~11h have good inhibitory activity against pancreatic cancer cell line BxPC-3, and 11e is the most potent compound with an IC50 value of 2.28μmol/L. 11e was observed to have no/low activity to other tested cancer cell lines and human normal liver cell line HL-7702, indicating that it is not a cytotoxic compound. Overall, 11e may be a good hit compound for further efforts to develop new inhibitors against pancreatic cancer.
Study on new anticancer drugs is one of the key tasks of global drug development. We previously found that 3, 5-disubstituted-1H-indole derivatives have apparent inhibitory activity against pancreatic cancer cells. Here we reported a new simple and efficient route for the synthesis of 3-((substituted-thio)methyl)-5-acylamino-1H-indole derivatives, which involves Vilsmeier-Haack reaction, Boc protection of secondary amine, aldehyde reduction, carboxylic acid and amine condensation reaction, and eight new target compounds (11a~11h) were synthesized. The cell-based assays revealed that 11a~11h have good inhibitory activity against pancreatic cancer cell line BxPC-3, and 11e is the most potent compound with an IC50 value of 2.28μmol/L. 11e was observed to have no/low activity to other tested cancer cell lines and human normal liver cell line HL-7702, indicating that it is not a cytotoxic compound. Overall, 11e may be a good hit compound for further efforts to develop new inhibitors against pancreatic cancer.
2018, 81(5): 461-465
Abstract:
Dihydropyrazole, a five-membered heterocyclic molecule, is an important organic compound with a broad range of biological activities. In this study, nine new 3-aryl-5-(furan-2-yl)-4, 5-dihydro-1H-pyrazole derivatives have been synthesized, and their in vitro anti-inflammatory and antioxidant activities were evaluated in lipopolysaccharide (LPS)-stimulated RAW-264.7 macrophages and DPPH model, respectively. The structures were characterized by IR, 1H NMR and 13C NMR. The biological results demonstrated that the amide compounds showed potential anti-inflammatory and antioxidant activity. In particular, compounds 4b and 4c were found to be similar anti-inflammatory to positive control dexamethasone (IC50=7.84μmol/L and 10.52μmol/L, respectively), and DPPH free radical scavenging rate of compound 3, 4b, 4c and 4d was up to 90% (4mg/mL).
Dihydropyrazole, a five-membered heterocyclic molecule, is an important organic compound with a broad range of biological activities. In this study, nine new 3-aryl-5-(furan-2-yl)-4, 5-dihydro-1H-pyrazole derivatives have been synthesized, and their in vitro anti-inflammatory and antioxidant activities were evaluated in lipopolysaccharide (LPS)-stimulated RAW-264.7 macrophages and DPPH model, respectively. The structures were characterized by IR, 1H NMR and 13C NMR. The biological results demonstrated that the amide compounds showed potential anti-inflammatory and antioxidant activity. In particular, compounds 4b and 4c were found to be similar anti-inflammatory to positive control dexamethasone (IC50=7.84μmol/L and 10.52μmol/L, respectively), and DPPH free radical scavenging rate of compound 3, 4b, 4c and 4d was up to 90% (4mg/mL).
2018, 81(5): 466-471
Abstract:
A kind of diamino-phthalonitrile (DPN) monomer was successfully synthesized. The chemical structures of DPN and its intermediate (DHTM, a phenol that contain two amino groups) were confirmed by spectroscopic techniques. Differential scanning calorimetry was utilized to demonstrate the autocatalytic performance of DPN and its curing effect on epoxy resin (EP). Blends of DHTM and DPN with EP were obtained, respectively. The thermal stabilities and dynamic mechanical properties of cured resins were studied by thermo-gravimetric and dynamic mechanical analysis. The results showed that all properties of DPN-EP cured resin are superior to DHTM-EP cured resin. For the former, the temperatures of 5% weight loss are 357 and 369℃ under nitrogen and air, respectively, and the glass temperature is 202℃. The limiting oxygen index is 36.36 calculate by Van Krevelen equation. The DPN-EP cured resin will be a great candidate as a matrix for high-performance polymeric material.
A kind of diamino-phthalonitrile (DPN) monomer was successfully synthesized. The chemical structures of DPN and its intermediate (DHTM, a phenol that contain two amino groups) were confirmed by spectroscopic techniques. Differential scanning calorimetry was utilized to demonstrate the autocatalytic performance of DPN and its curing effect on epoxy resin (EP). Blends of DHTM and DPN with EP were obtained, respectively. The thermal stabilities and dynamic mechanical properties of cured resins were studied by thermo-gravimetric and dynamic mechanical analysis. The results showed that all properties of DPN-EP cured resin are superior to DHTM-EP cured resin. For the former, the temperatures of 5% weight loss are 357 and 369℃ under nitrogen and air, respectively, and the glass temperature is 202℃. The limiting oxygen index is 36.36 calculate by Van Krevelen equation. The DPN-EP cured resin will be a great candidate as a matrix for high-performance polymeric material.
2018, 81(5): 472-475
Abstract:
Enzyme is an important active substance in nature, its structures and properties are easily affected by the external environment. Now it is one of the hot topics in the research to increase and maintain enzyme activity. In this paper, pepsin was used as a model to study the effect of zwitterionic compounds such as methacryloyloxyethyl phosphorylcholine (MPC), sulfobetaine methacrylate (SBMA), carboxybetaine methacrylate (CBMA) on pepsin activity. The results showed that the pepsin activity in the presence of CBMA was 453% of the control after 2h at 60℃, and still 330% of the control pepsin after 6 h at 60℃. CBMA could significantly increase pepsin activity.
Enzyme is an important active substance in nature, its structures and properties are easily affected by the external environment. Now it is one of the hot topics in the research to increase and maintain enzyme activity. In this paper, pepsin was used as a model to study the effect of zwitterionic compounds such as methacryloyloxyethyl phosphorylcholine (MPC), sulfobetaine methacrylate (SBMA), carboxybetaine methacrylate (CBMA) on pepsin activity. The results showed that the pepsin activity in the presence of CBMA was 453% of the control after 2h at 60℃, and still 330% of the control pepsin after 6 h at 60℃. CBMA could significantly increase pepsin activity.
2018, 81(5): 476-479
Abstract:
An efficient access to vinylboronates was achieved through (NHC)CuCl-catalyzed hydroboration of symmetric internal alkynes. With bis(pinacolato)diboron and symmetric internal alkynes as starting materials, single configuration of vinylboronates were obtained after protonation of vinylcopper, and their structure were all determined by 1H NMR, 13C NMR and HRMS. The optimal reaction conditions were systematically screened. Based on the reaction investigation, the possible reaction mechanism was discussed. This highly practical hydroboration process, which can be carried out at mild conditions, enjoys operational simplicity, as well as environmental benign catalyst.
An efficient access to vinylboronates was achieved through (NHC)CuCl-catalyzed hydroboration of symmetric internal alkynes. With bis(pinacolato)diboron and symmetric internal alkynes as starting materials, single configuration of vinylboronates were obtained after protonation of vinylcopper, and their structure were all determined by 1H NMR, 13C NMR and HRMS. The optimal reaction conditions were systematically screened. Based on the reaction investigation, the possible reaction mechanism was discussed. This highly practical hydroboration process, which can be carried out at mild conditions, enjoys operational simplicity, as well as environmental benign catalyst.
