Two coordination polymers constructed from 3,4-thiophenedicarboxylic acid and bis（2-methyl imidazole） ligands, namely, {[Cd2（tdc）2（bip）2]·7H20}n （1） and [Cd（tdc）（bib）]n （2） （Hgtdc = 3,4-thiophenedi...Two coordination polymers constructed from 3,4-thiophenedicarboxylic acid and bis（2-methyl imidazole） ligands, namely, {[Cd2（tdc）2（bip）2]·7H20}n （1） and [Cd（tdc）（bib）]n （2） （Hgtdc = 3,4-thiophenedicarboxylic acid, bip = 1,3-bis-（imidazol-2-methyl）propane and bib = 1,4-bis（imidazol-2-methyl）butane）, have been synthesized and structurally characterized by single-crystal X-ray diffraction. Structural analyses reveal that 1 exhibits a two-dimensional （2D） layered network with 3-connected （6,3） topology, which is further connected into a three- dimensional （3D） supramolecular structure by intermolecular hydrogen bonds. However, 2 features a 2D network which can be rationalized as a 4-connected sql net. The results indicate the subtle difference of auxiliary bis（imidazol-2-methyl） ligands may lead to diverse architectures. Moreover, they exhibit luminescence emission in the solid state at room temperature.展开更多
As a prevailing cathode material of lithium-ion batteries(LIBs),LiCoO_(2)(LCO)still encounters the tricky problems of structural collapse,whose morphological engineering and cation doping are crucial for surmounting t...As a prevailing cathode material of lithium-ion batteries(LIBs),LiCoO_(2)(LCO)still encounters the tricky problems of structural collapse,whose morphological engineering and cation doping are crucial for surmounting the mechanical strains and alleviating phase degradation upon cycling.Hereinafter,we propose a strategy using a zeolitic imidazolate framework(ZIF)as the self-sacrificing template to directionally prepare a series of LiNi_(0.1)Co_(0.9)O_(2)(LNCO)with tailorable electrochemical properties.The rational selection of sintering temperature imparts the superiority of the resultant products in lithium storage,during which the sample prepared at 700℃(LNCO-700)outperforms its counterparts in cyclability(156.8 mA h g^(-1)at 1 C for 200 cycles in half cells,1 C=275 mA g^(-1))and rate capability due to the expedited ion/electron transport and the strengthen mechanical robustness.The feasibility of proper Ni doping is also divulged by half/full cell tests and theoretical study,during which LNCO-700(167 mA h g^(-1)at 1 C for 100 cycles in full cells)surpasses LCO-700 in battery performance due to the mitigated phase deterioration,stabilized layered structu re,ameliorated electro nic co nductivity,a nd exalted lithium sto rage activity.This work systematically unveils tailorable electrochemical behaviors of LNCO to better direct their practical application.展开更多
The title complex [Na（H2MIA-）（H2O）]（1,H3MIA = 2-methyl-1H-imidazole-4,5-dicarboxylic acid） has been synthesized by hydrothermal synthesis and structurally characterized by X-ray crystallography.Compound 1 crysta...The title complex [Na（H2MIA-）（H2O）]（1,H3MIA = 2-methyl-1H-imidazole-4,5-dicarboxylic acid） has been synthesized by hydrothermal synthesis and structurally characterized by X-ray crystallography.Compound 1 crystallizes in orthorhombic,space group ibam with a = 14.4737（19）,b = 17.553（2）,c = 6.5285（9）,V = 1658.6（4） 3,C6H7N2NaO5,Mr = 210.12,Z = 8,Dc = 1.675 g/cm3,F（000） = 864,μ = 0.188 mm-1,λ（MoKα） = 0.071073 ,R = 0.0383 and wR = 0.0987 for 1046 observed reflections（I 2σ（I））.In the structure of 1,each coordination water coordinates with two Na（I） ions at the same time and links the neighboring Na（I） ions to form a one-dimensional Na（I）-water chain.Each H2MIA-ligand links the neighboring Na（I） of Na（I）-water chain to form a novel two-dimensional supramolecular network.The 2-D network is stabilized by O-H…N hydrogen bonds and π-π interaction.The 2D network is further linked via O-H…O hydrogen bonds to yield a three-dimensional framework.展开更多
A novel one-pot synthesis of 4,5-bis(hydroxymethyl) imidazoles 2a-b, new ethers 3a-b and a new type of imidazolophane 4b by the bis-hydroxymethylation of imidazole or 2-methyl imidazole with formaldehyde and potassium...A novel one-pot synthesis of 4,5-bis(hydroxymethyl) imidazoles 2a-b, new ethers 3a-b and a new type of imidazolophane 4b by the bis-hydroxymethylation of imidazole or 2-methyl imidazole with formaldehyde and potassium hydroxide is reported. The structures of these compounds have been established by MS, (1)HNMR IR and elemental analyses.展开更多
Layered assembled membranes of 2D leaf-like zeolitic imidazolate frameworks(ZIF-L)nanosheets have received great attention in the field of water treatment due to the porous structure and excellent antibacterial abilit...Layered assembled membranes of 2D leaf-like zeolitic imidazolate frameworks(ZIF-L)nanosheets have received great attention in the field of water treatment due to the porous structure and excellent antibacterial ability,but the dense accumulation on the membrane surface and the low permeate flux greatly hinder their application.Herein,we synthesized m HNTs(modified halloysite nanotubes)/ZIF-L nanocomposites on modified m HNTs by in situ growth method.Interestingly,due to the different size of m HNTs and ZIF-L,m HNTs were packed in ZIF-L nanosheets.The hollow m HNTs provided additional transport channels for water molecules,and the accumulation of the ZIF-L nanosheets was decreased after assembling m HNTs/ZIF-L nanocomposites into membrane by filtration.The prepared m HNTs/ZIF-L membrane presented high permeate flux(59.6 L·m^(-2)·h^(-1)),which is 2-4 times of the ZIF-L membranes(14.8 L·m^(-2)·h^(-1)).Moreover,m HNTs/ZIF-L membranes are intrinsically antimicrobial,which exhibit extremely high bacterial resistance.We provide a controllable strategy to improve 2D ZIF-L assembles,and develops novel membranes using 2D package structure as building units.展开更多
A simple, convenient and efficient method for the synthesis of 1,2,4,5-tetrasubstituted imidazole derivatives using benzoin, an aromatic aldehyde, an aromatic amine in the presence of ammonium acetate catalyzed by hig...A simple, convenient and efficient method for the synthesis of 1,2,4,5-tetrasubstituted imidazole derivatives using benzoin, an aromatic aldehyde, an aromatic amine in the presence of ammonium acetate catalyzed by high surface area SiO2 and induced by free solar thermal energy was reported. C 2009 Kamal User Sadek. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.展开更多
A novel method for synthesis of 2-butyl-5 -chloro-3H-imidazole-4-carbaldehyde 2, a key intermediate of Losartan was reported. The compound 2 was synthesized from starting material dimethyl malonate 6 and n-valeronitri...A novel method for synthesis of 2-butyl-5 -chloro-3H-imidazole-4-carbaldehyde 2, a key intermediate of Losartan was reported. The compound 2 was synthesized from starting material dimethyl malonate 6 and n-valeronitrile 8 by six steps with an overall yield of 40%. The key step including the reaction of compound 5 with POCl3/DMF followed by hydrolysis to give compound 2 with the yield of 68%.展开更多
A new Cd（Ⅱ） complex（[Cd（H2PIDC）2]n） with singly deprotonated 2-propyl-imidazole-4,5-dicarboxylate as bridging ligand was synthesized and characterized by X-ray diffraction method.Crystal data：monoclinic,space ...A new Cd（Ⅱ） complex（[Cd（H2PIDC）2]n） with singly deprotonated 2-propyl-imidazole-4,5-dicarboxylate as bridging ligand was synthesized and characterized by X-ray diffraction method.Crystal data：monoclinic,space group P21/c,with a=8.2547（11）,b=10.7071（15）,c=13.9131（14）A,β=126.164（5）o,V=992.8（2）A^3,C16H18N4O8Cd,Mr=506.74,Z=2,Dc=1.695g/cm^3,F（000）=508,μ=1.151 mm^-1,R=0.0296 and wR=0.0812 for 1581 observed reflections.Singly deprotonated ligands（H2PIDC-） act as μ3-bridge and join the Cd（Ⅱ） atoms into a 2-D layer structure.The 2-D layers are further linked by intermolecular hydrogen bonds into a 3D network.The luminescent property of the complex was also investigated.展开更多
A simple and efficient method has been developed;benzil/benzoin undergoes smooth condensation with various substituted aldehyde and ammonium acetate in the presence of potassium dihydrogen phosphate（KH;PO;） under mi...A simple and efficient method has been developed;benzil/benzoin undergoes smooth condensation with various substituted aldehyde and ammonium acetate in the presence of potassium dihydrogen phosphate（KH;PO;） under mild reaction conditions to afford the corresponding trisubstituted imidazole in excellent yields.The method for synthesis of product,the reaction mixture was reflux in ethanol for 40-90 min.The present method is simple,efficient,and cost-effective.展开更多
A new Gd coordination polymer based on 2-（pyridin-3-yl）-lH-imidazole-4,5-dicar- boxylate, formulated as {[Gd2（HPyIDC）2（H2O）5]·（bpy）·（NO3）2·3H2O}n （1, bpy = 4,4＇-bipyridine） has been synthes...A new Gd coordination polymer based on 2-（pyridin-3-yl）-lH-imidazole-4,5-dicar- boxylate, formulated as {[Gd2（HPyIDC）2（H2O）5]·（bpy）·（NO3）2·3H2O}n （1, bpy = 4,4＇-bipyridine） has been synthesized under hydrothermal conditions. The compound crystallizes in triclinic, space group Pi with a = 11.451（2）, b = 11.596（2）, c = 15.7333（3） A, β = 79.47（3）°, Z = 2, V= 1948.6（7） A^3, C30H34Gd2N10O22, Dc = 2.047 g/cm^3, Mr= 1201.17, 2（MoKa） = 0.71073 A,μ = 3.477 mml, F（000） = 1176, the final R = 0.0554 and wR = 0.1181. Polymer 1 is a 2D network built up from 4-connected HPylDC2- anion and 4-connected Gd ions. Dielectric constant of complex 1 was measured at different frequencies with temperature variation.展开更多
t 4,5 -diphenyl, 4,5 - bis(4 - methylphenyl), 4,5 - bis(4 - methoxyphenyl) - 2 -(2,5 - dAnethylthiophen -3 -yl ) imidazoles were synthesized. Oxidation of the obtained Anidazoles with potassium ferricyanide in water -...t 4,5 -diphenyl, 4,5 - bis(4 - methylphenyl), 4,5 - bis(4 - methoxyphenyl) - 2 -(2,5 - dAnethylthiophen -3 -yl ) imidazoles were synthesized. Oxidation of the obtained Anidazoles with potassium ferricyanide in water - alcohol solution of alkali gave the corresponding dimers. The structtires of imidazoles were characterized by IR, 1H NMR, mass spectroscopy and elemental analysis. The structures of dimers were characterized by IR, elemental analysis and chromatography展开更多
Application of sulfuric acid immobilized on silica gel as an efficient and benign catalyst has been explored in the syn-thesis of 2,4,5-Triaryl-1H-imidazoles via condensation reaction of benzil or benzoin, aldehyde an...Application of sulfuric acid immobilized on silica gel as an efficient and benign catalyst has been explored in the syn-thesis of 2,4,5-Triaryl-1H-imidazoles via condensation reaction of benzil or benzoin, aldehyde and ammonium acetate. The key advantages of this process are high yields, cost effectiveness of catalyst, easy work-up, purification of products by non-chromatographic method and the reusability of the H2SO4.SiO2 catalyst.展开更多
In the last few decades,nitroimidazoles have been investigated mostly due to their properties as antibiotics,radiosensitizers and anti-protozoans[1 -3].Recently these nitroimidazoles,such as 2,4-dinitroimidazole,1-met...In the last few decades,nitroimidazoles have been investigated mostly due to their properties as antibiotics,radiosensitizers and anti-protozoans[1 -3].Recently these nitroimidazoles,such as 2,4-dinitroimidazole,1-methyl-2,4,5-trinitroimidazole and their energetic salts, have attracted renewed attention for their favorable explosive performance as well as improved safety characteristics[4,5].Because of the activity of cyano group,2-nitro-4,5-dicyano-1 H-imidazole (NDCI) could be used as an intermediate in the synthesis of novel energetic materials containing nitroimidazole moiety.NDCI has been synthesized by the procedure given by Yixin Lu and coworkers[6],where the diazotization reaction and the Sandmeyer reaction were separately achieved.NDCI was obtained by adding a solution of sodium nitrite to 2-diazo4,5-dicyanoimidazole which was generated by diazotization of 2-amino-4,5-dicyano-1H-imidazole ( ADCI ) with sodium nitrite in water-hydrochloric acid and collected by filtration.Dry 2-diazo-4,5-dicyanoimidazole was so sensitive to shock that its separation may cause explosion[7].展开更多
The reaction of imidazole-2-thione derivative 1 with 2-chloro-N-p-tolylacetamide afforded the corresponding 2-(1HI-imidazol-2-ylthio)-N-p-tolylacetamide 2. Reaction compound 2 with different reagents such as p-chlorob...The reaction of imidazole-2-thione derivative 1 with 2-chloro-N-p-tolylacetamide afforded the corresponding 2-(1HI-imidazol-2-ylthio)-N-p-tolylacetamide 2. Reaction compound 2 with different reagents such as p-chlorobenzaldehyde and p-chlorophenyl diazonium chloride afforded the corresponding arylidene derivative 3 and hydrazone derivative 6. Reactions of 2 with carbon disulfide in dimethylformamide (DMF) in one equivalent potassium hydroxide afforded intermediate potassium sulphide salt 8, which treatment with dilute hydrochloric acid and phenacyl bromide afforded the corresponding 2-[p-tolylcarbamoyl]ethanedithioic acid 9 and 3-[benzo-ylmethylthio]-N-p-tolyl-3-thioxo-propaneamide 10. While the reaction 2 with carbon disulphide in the presence of two equivalent potassium hydroxide in DMF gave non-isolated potassium salt 11, which was allowed to react with halogenated compounds namely ethyl chloroacetate and methyl iodide afforded the corresponding 3, 3-bis[(ethoxycarbonyl)methylthio]-N-p-tolylacrylamide 12 and 3,3-bis-(methylthio)-N-p-tolylacrylamide 13 respectively. Reaction 2 with phenyl isothiocyanate in basic DMF yielded the intermediate potassium sulphide salt 18. Acidification 18 with dilute hydro-chloric acid afforded the corresponding thiocarbamoyl derivative 19. Treatment of intermediate 18 with methyl iodide, phenacyl bromide and ethylchloroacetate afforded the 3-anilino-3-(methylthio)-N-p-tolylacrylamide 20, 2-(1,3-thiazol-2(3H)-ylidene)-N-p-tolylacetamide 21 and 2-(4-oxo-3-phenyl-1,3-thiazolidin-2-ylidene)-N-p-tolylacetamide 22 respectively. The structure of the newly synthesized compounds has been confirmed by elemental analysis and spectra data. Synthesized compounds 2, 3, 6, 13, 15a, 15b, 17, 20, 21, 22 and 23 were screened for their antibacterial activities in vitro against Gram-positive (Staphylococcus aureus and Bacillus subtilis), Gram-negative (Pseudomonas aeuroginosa and Escherichia coli ) and antifungal activities against (Aspergillus fumigates, Syncephalastrum racemosum, Geotrichum candidum and Candida albicans).展开更多
基金supported by the National Natural Science of Foundation of China(No.21305060)
文摘Two coordination polymers constructed from 3,4-thiophenedicarboxylic acid and bis（2-methyl imidazole） ligands, namely, {[Cd2（tdc）2（bip）2]·7H20}n （1） and [Cd（tdc）（bib）]n （2） （Hgtdc = 3,4-thiophenedicarboxylic acid, bip = 1,3-bis-（imidazol-2-methyl）propane and bib = 1,4-bis（imidazol-2-methyl）butane）, have been synthesized and structurally characterized by single-crystal X-ray diffraction. Structural analyses reveal that 1 exhibits a two-dimensional （2D） layered network with 3-connected （6,3） topology, which is further connected into a three- dimensional （3D） supramolecular structure by intermolecular hydrogen bonds. However, 2 features a 2D network which can be rationalized as a 4-connected sql net. The results indicate the subtle difference of auxiliary bis（imidazol-2-methyl） ligands may lead to diverse architectures. Moreover, they exhibit luminescence emission in the solid state at room temperature.
基金the financial support from the Special Funds for the Cultivation of Guangdong College Students’Scientific and Technological Innovation(“Climbing Program”Special Funds,pdjh2023b0145)Guangdong Provincial International Joint Research Center for Energy Storage Materials(2023A0505090009)。
文摘As a prevailing cathode material of lithium-ion batteries(LIBs),LiCoO_(2)(LCO)still encounters the tricky problems of structural collapse,whose morphological engineering and cation doping are crucial for surmounting the mechanical strains and alleviating phase degradation upon cycling.Hereinafter,we propose a strategy using a zeolitic imidazolate framework(ZIF)as the self-sacrificing template to directionally prepare a series of LiNi_(0.1)Co_(0.9)O_(2)(LNCO)with tailorable electrochemical properties.The rational selection of sintering temperature imparts the superiority of the resultant products in lithium storage,during which the sample prepared at 700℃(LNCO-700)outperforms its counterparts in cyclability(156.8 mA h g^(-1)at 1 C for 200 cycles in half cells,1 C=275 mA g^(-1))and rate capability due to the expedited ion/electron transport and the strengthen mechanical robustness.The feasibility of proper Ni doping is also divulged by half/full cell tests and theoretical study,during which LNCO-700(167 mA h g^(-1)at 1 C for 100 cycles in full cells)surpasses LCO-700 in battery performance due to the mitigated phase deterioration,stabilized layered structu re,ameliorated electro nic co nductivity,a nd exalted lithium sto rage activity.This work systematically unveils tailorable electrochemical behaviors of LNCO to better direct their practical application.
基金supported by the Research Foundation of Educational Department of Jiangxi Province (GJJ10421)the Natural Science Foundation of Jiangxi Agricultural University (09003321)
文摘The title complex [Na（H2MIA-）（H2O）]（1,H3MIA = 2-methyl-1H-imidazole-4,5-dicarboxylic acid） has been synthesized by hydrothermal synthesis and structurally characterized by X-ray crystallography.Compound 1 crystallizes in orthorhombic,space group ibam with a = 14.4737（19）,b = 17.553（2）,c = 6.5285（9）,V = 1658.6（4） 3,C6H7N2NaO5,Mr = 210.12,Z = 8,Dc = 1.675 g/cm3,F（000） = 864,μ = 0.188 mm-1,λ（MoKα） = 0.071073 ,R = 0.0383 and wR = 0.0987 for 1046 observed reflections（I 2σ（I））.In the structure of 1,each coordination water coordinates with two Na（I） ions at the same time and links the neighboring Na（I） ions to form a one-dimensional Na（I）-water chain.Each H2MIA-ligand links the neighboring Na（I） of Na（I）-water chain to form a novel two-dimensional supramolecular network.The 2-D network is stabilized by O-H…N hydrogen bonds and π-π interaction.The 2D network is further linked via O-H…O hydrogen bonds to yield a three-dimensional framework.
文摘A novel one-pot synthesis of 4,5-bis(hydroxymethyl) imidazoles 2a-b, new ethers 3a-b and a new type of imidazolophane 4b by the bis-hydroxymethylation of imidazole or 2-methyl imidazole with formaldehyde and potassium hydroxide is reported. The structures of these compounds have been established by MS, (1)HNMR IR and elemental analyses.
基金supported by the Excellent Youth Foundation of Henan Scientific Committee,China(222300420018)Key Scientific Research Projects in Universities of Henan Province,China(21zx006)。
文摘Layered assembled membranes of 2D leaf-like zeolitic imidazolate frameworks(ZIF-L)nanosheets have received great attention in the field of water treatment due to the porous structure and excellent antibacterial ability,but the dense accumulation on the membrane surface and the low permeate flux greatly hinder their application.Herein,we synthesized m HNTs(modified halloysite nanotubes)/ZIF-L nanocomposites on modified m HNTs by in situ growth method.Interestingly,due to the different size of m HNTs and ZIF-L,m HNTs were packed in ZIF-L nanosheets.The hollow m HNTs provided additional transport channels for water molecules,and the accumulation of the ZIF-L nanosheets was decreased after assembling m HNTs/ZIF-L nanocomposites into membrane by filtration.The prepared m HNTs/ZIF-L membrane presented high permeate flux(59.6 L·m^(-2)·h^(-1)),which is 2-4 times of the ZIF-L membranes(14.8 L·m^(-2)·h^(-1)).Moreover,m HNTs/ZIF-L membranes are intrinsically antimicrobial,which exhibit extremely high bacterial resistance.We provide a controllable strategy to improve 2D ZIF-L assembles,and develops novel membranes using 2D package structure as building units.
文摘A simple, convenient and efficient method for the synthesis of 1,2,4,5-tetrasubstituted imidazole derivatives using benzoin, an aromatic aldehyde, an aromatic amine in the presence of ammonium acetate catalyzed by high surface area SiO2 and induced by free solar thermal energy was reported. C 2009 Kamal User Sadek. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.
基金supported by Outstanding Youth Foundation of Heilongjiang Province(No.JC200706)
文摘A novel method for synthesis of 2-butyl-5 -chloro-3H-imidazole-4-carbaldehyde 2, a key intermediate of Losartan was reported. The compound 2 was synthesized from starting material dimethyl malonate 6 and n-valeronitrile 8 by six steps with an overall yield of 40%. The key step including the reaction of compound 5 with POCl3/DMF followed by hydrolysis to give compound 2 with the yield of 68%.
基金supported by the National Natural Science Foundation of China (No 20771054)the Foundation of Education Committee of Henan Province (2006150017)
文摘A new Cd（Ⅱ） complex（[Cd（H2PIDC）2]n） with singly deprotonated 2-propyl-imidazole-4,5-dicarboxylate as bridging ligand was synthesized and characterized by X-ray diffraction method.Crystal data：monoclinic,space group P21/c,with a=8.2547（11）,b=10.7071（15）,c=13.9131（14）A,β=126.164（5）o,V=992.8（2）A^3,C16H18N4O8Cd,Mr=506.74,Z=2,Dc=1.695g/cm^3,F（000）=508,μ=1.151 mm^-1,R=0.0296 and wR=0.0812 for 1581 observed reflections.Singly deprotonated ligands（H2PIDC-） act as μ3-bridge and join the Cd（Ⅱ） atoms into a 2-D layer structure.The 2-D layers are further linked by intermolecular hydrogen bonds into a 3D network.The luminescent property of the complex was also investigated.
文摘A simple and efficient method has been developed;benzil/benzoin undergoes smooth condensation with various substituted aldehyde and ammonium acetate in the presence of potassium dihydrogen phosphate（KH;PO;） under mild reaction conditions to afford the corresponding trisubstituted imidazole in excellent yields.The method for synthesis of product,the reaction mixture was reflux in ethanol for 40-90 min.The present method is simple,efficient,and cost-effective.
基金Supported by the National Natural Science Foundation of China(No.21201087)Jiangsu Province NSF BK20131244+1 种基金the Foundation of Jiangsu Educational Committee(11KJB150004)Qing Lan Project of Jiangsu Province
文摘A new Gd coordination polymer based on 2-（pyridin-3-yl）-lH-imidazole-4,5-dicar- boxylate, formulated as {[Gd2（HPyIDC）2（H2O）5]·（bpy）·（NO3）2·3H2O}n （1, bpy = 4,4＇-bipyridine） has been synthesized under hydrothermal conditions. The compound crystallizes in triclinic, space group Pi with a = 11.451（2）, b = 11.596（2）, c = 15.7333（3） A, β = 79.47（3）°, Z = 2, V= 1948.6（7） A^3, C30H34Gd2N10O22, Dc = 2.047 g/cm^3, Mr= 1201.17, 2（MoKa） = 0.71073 A,μ = 3.477 mml, F（000） = 1176, the final R = 0.0554 and wR = 0.1181. Polymer 1 is a 2D network built up from 4-connected HPylDC2- anion and 4-connected Gd ions. Dielectric constant of complex 1 was measured at different frequencies with temperature variation.
文摘t 4,5 -diphenyl, 4,5 - bis(4 - methylphenyl), 4,5 - bis(4 - methoxyphenyl) - 2 -(2,5 - dAnethylthiophen -3 -yl ) imidazoles were synthesized. Oxidation of the obtained Anidazoles with potassium ferricyanide in water - alcohol solution of alkali gave the corresponding dimers. The structtires of imidazoles were characterized by IR, 1H NMR, mass spectroscopy and elemental analysis. The structures of dimers were characterized by IR, elemental analysis and chromatography
文摘Application of sulfuric acid immobilized on silica gel as an efficient and benign catalyst has been explored in the syn-thesis of 2,4,5-Triaryl-1H-imidazoles via condensation reaction of benzil or benzoin, aldehyde and ammonium acetate. The key advantages of this process are high yields, cost effectiveness of catalyst, easy work-up, purification of products by non-chromatographic method and the reusability of the H2SO4.SiO2 catalyst.
文摘In the last few decades,nitroimidazoles have been investigated mostly due to their properties as antibiotics,radiosensitizers and anti-protozoans[1 -3].Recently these nitroimidazoles,such as 2,4-dinitroimidazole,1-methyl-2,4,5-trinitroimidazole and their energetic salts, have attracted renewed attention for their favorable explosive performance as well as improved safety characteristics[4,5].Because of the activity of cyano group,2-nitro-4,5-dicyano-1 H-imidazole (NDCI) could be used as an intermediate in the synthesis of novel energetic materials containing nitroimidazole moiety.NDCI has been synthesized by the procedure given by Yixin Lu and coworkers[6],where the diazotization reaction and the Sandmeyer reaction were separately achieved.NDCI was obtained by adding a solution of sodium nitrite to 2-diazo4,5-dicyanoimidazole which was generated by diazotization of 2-amino-4,5-dicyano-1H-imidazole ( ADCI ) with sodium nitrite in water-hydrochloric acid and collected by filtration.Dry 2-diazo-4,5-dicyanoimidazole was so sensitive to shock that its separation may cause explosion[7].
文摘The reaction of imidazole-2-thione derivative 1 with 2-chloro-N-p-tolylacetamide afforded the corresponding 2-(1HI-imidazol-2-ylthio)-N-p-tolylacetamide 2. Reaction compound 2 with different reagents such as p-chlorobenzaldehyde and p-chlorophenyl diazonium chloride afforded the corresponding arylidene derivative 3 and hydrazone derivative 6. Reactions of 2 with carbon disulfide in dimethylformamide (DMF) in one equivalent potassium hydroxide afforded intermediate potassium sulphide salt 8, which treatment with dilute hydrochloric acid and phenacyl bromide afforded the corresponding 2-[p-tolylcarbamoyl]ethanedithioic acid 9 and 3-[benzo-ylmethylthio]-N-p-tolyl-3-thioxo-propaneamide 10. While the reaction 2 with carbon disulphide in the presence of two equivalent potassium hydroxide in DMF gave non-isolated potassium salt 11, which was allowed to react with halogenated compounds namely ethyl chloroacetate and methyl iodide afforded the corresponding 3, 3-bis[(ethoxycarbonyl)methylthio]-N-p-tolylacrylamide 12 and 3,3-bis-(methylthio)-N-p-tolylacrylamide 13 respectively. Reaction 2 with phenyl isothiocyanate in basic DMF yielded the intermediate potassium sulphide salt 18. Acidification 18 with dilute hydro-chloric acid afforded the corresponding thiocarbamoyl derivative 19. Treatment of intermediate 18 with methyl iodide, phenacyl bromide and ethylchloroacetate afforded the 3-anilino-3-(methylthio)-N-p-tolylacrylamide 20, 2-(1,3-thiazol-2(3H)-ylidene)-N-p-tolylacetamide 21 and 2-(4-oxo-3-phenyl-1,3-thiazolidin-2-ylidene)-N-p-tolylacetamide 22 respectively. The structure of the newly synthesized compounds has been confirmed by elemental analysis and spectra data. Synthesized compounds 2, 3, 6, 13, 15a, 15b, 17, 20, 21, 22 and 23 were screened for their antibacterial activities in vitro against Gram-positive (Staphylococcus aureus and Bacillus subtilis), Gram-negative (Pseudomonas aeuroginosa and Escherichia coli ) and antifungal activities against (Aspergillus fumigates, Syncephalastrum racemosum, Geotrichum candidum and Candida albicans).
