A new method for synthesizing 5-chloro-1-methyl-4-nitroimidazole had been devoloped with diethyl oxalate,aqueous methylamine formate,phosphorus pentachloride,mixed acid etc as starting materials.Target molecule was ob...A new method for synthesizing 5-chloro-1-methyl-4-nitroimidazole had been devoloped with diethyl oxalate,aqueous methylamine formate,phosphorus pentachloride,mixed acid etc as starting materials.Target molecule was obtained through aminolysis reaction,semi-ring reaction and nitration reaction.The process provided an energy saving,high yield synthetic methodology.The yield of producing 5-chloro-1-methyl-4-nitroimidazole was up to 64%.All products were determined by MS,NMR and FT-IR.展开更多
The reaction of 2,6-diformyl-4-methylphenol, ethylenediamine and Cu（Ⅱ） in the proportion of 3：2：2 yields a new tetranuclear copper（Ⅱ） complex, [Cu2L]2（ClO4）2.2H2O（H3L= N,N＇-bis（4-（3＇-formyl-5＇-methylsa...The reaction of 2,6-diformyl-4-methylphenol, ethylenediamine and Cu（Ⅱ） in the proportion of 3：2：2 yields a new tetranuclear copper（Ⅱ） complex, [Cu2L]2（ClO4）2.2H2O（H3L= N,N＇-bis（4-（3＇-formyl-5＇-methylsalicyclidene）iminoethyl）-4-methyl-2,6-bimethyliminophenol）. The complex has been characterized by ES-MS, IR and X-ray diffraction analysis, and its crystal crystallizes in the triclinic system, space group P1 with a = 10.8673（11）, b = 12.0829（12）, c = 14.4834（15） А, α= 111.946（2）, β= 105.828（2）, γ = 99.583（2）°,V= 1618.5（3） А^3, Dc = 1.605 g/cm^3, Z = 2, Mr = 1564.26, F（000） = 800.0,μ（MoKa） = 1.460/mm, S = 1.063, R = 0.0612 and wR = 0.1163 for 6245 observed reflections （I 〉 2σ（I））. The complex is a dimer of dinuclear copper（Ⅱ） acylic enantiomorph subunit [Cu2L]ClO4.H_2O, held together by π…π weak coordination and hydrogen bonding interactions. In addition, the π…π interactions related to phenyl moieties as well as CH=N…π interactions were also found to stabilize the supramolecular architectures in the solid state.展开更多
文摘A new method for synthesizing 5-chloro-1-methyl-4-nitroimidazole had been devoloped with diethyl oxalate,aqueous methylamine formate,phosphorus pentachloride,mixed acid etc as starting materials.Target molecule was obtained through aminolysis reaction,semi-ring reaction and nitration reaction.The process provided an energy saving,high yield synthetic methodology.The yield of producing 5-chloro-1-methyl-4-nitroimidazole was up to 64%.All products were determined by MS,NMR and FT-IR.
基金Supported by the key Foundation of the Education Department of Hubei Province (No. D20081503)the foundation of the innovative group of the Education Department of Hubei Province (T200802)
文摘The reaction of 2,6-diformyl-4-methylphenol, ethylenediamine and Cu（Ⅱ） in the proportion of 3：2：2 yields a new tetranuclear copper（Ⅱ） complex, [Cu2L]2（ClO4）2.2H2O（H3L= N,N＇-bis（4-（3＇-formyl-5＇-methylsalicyclidene）iminoethyl）-4-methyl-2,6-bimethyliminophenol）. The complex has been characterized by ES-MS, IR and X-ray diffraction analysis, and its crystal crystallizes in the triclinic system, space group P1 with a = 10.8673（11）, b = 12.0829（12）, c = 14.4834（15） А, α= 111.946（2）, β= 105.828（2）, γ = 99.583（2）°,V= 1618.5（3） А^3, Dc = 1.605 g/cm^3, Z = 2, Mr = 1564.26, F（000） = 800.0,μ（MoKa） = 1.460/mm, S = 1.063, R = 0.0612 and wR = 0.1163 for 6245 observed reflections （I 〉 2σ（I））. The complex is a dimer of dinuclear copper（Ⅱ） acylic enantiomorph subunit [Cu2L]ClO4.H_2O, held together by π…π weak coordination and hydrogen bonding interactions. In addition, the π…π interactions related to phenyl moieties as well as CH=N…π interactions were also found to stabilize the supramolecular architectures in the solid state.
