The synthesis of 1,4,5,8-tetramethoxynaphthalene-2-carboxaldehyde,an intermediate of shikonin was investigated.1,4,5,8-tetramethoxynaphthalene was prepared from the oxidation of 1,5-dinitronaphthalene and the reaction...The synthesis of 1,4,5,8-tetramethoxynaphthalene-2-carboxaldehyde,an intermediate of shikonin was investigated.1,4,5,8-tetramethoxynaphthalene was prepared from the oxidation of 1,5-dinitronaphthalene and the reaction product naphthazarin was directly methylated without been purified.The title compound was obtained by the formylation of 1,4,5,8-tetramethoxynaphthalene.The overall yield was 38.5% based on 1,5-dinitronaphthalene.展开更多
A novel coordination polymer [Ba2(AQTC)(H2O)3]n(1, H4 AQTC = anthraquinone-1,4,5,8-tetracarboxylic acid) has been prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction, ele...A novel coordination polymer [Ba2(AQTC)(H2O)3]n(1, H4 AQTC = anthraquinone-1,4,5,8-tetracarboxylic acid) has been prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectroscopy and thermogravimetric analysis. Two quinone oxygen atoms and all carboxylate oxygen atoms of AQTC4- are involved in coordination. Two equivalent barium ions are mainly linked by carboxylate oxygen atoms into a dimer. Neighbouring dimers are further connected by the AQTC4- ligand through carboxylate oxygen atom, leading to a 1-D chain structure. Every two adjacent chains are mainly further connected by face carboxylate oxygen atoms and water molecule, generating a two-dimensional layer structure. Such 2-D layer structures are connected with O(6) and O(6C) atoms from water molecules to form a 3-D structure. In addition, luminescent properties of 1 are also investigated.展开更多
An experimental study was carried out on the direct nitration of 1,4,5,8-tetraaza-bicyclo-[4,4,0]-decane to synthesize 1,4,5,8-tetranitro-l,4,5,8-tetraazabicyclo-[4,4,0]-decane (TNAD) with N205 catalyzed by acidic i...An experimental study was carried out on the direct nitration of 1,4,5,8-tetraaza-bicyclo-[4,4,0]-decane to synthesize 1,4,5,8-tetranitro-l,4,5,8-tetraazabicyclo-[4,4,0]-decane (TNAD) with N205 catalyzed by acidic ionic liquids. Various ionic liquids, such as [HMim]X, [(CH2)4SO3HMim]X and [Capl]X (X =pTSO-, NO3 , HS04-), and various parameters such as equivalents of ionic liquid, molar ratio of N205 tO the starting material, reaction time and temperature, and solvent were investigated, Ionic liquid [(CH2)4SO3HMim]HS04 showed better catalytic activity. In the presence of 3% molar ratio of [(CH2)4SO3HMim]HS04 ionic liquid to the staring material, the yield of 1,4,5,8-tetranitro-l,4,5,8- tetraazabicvclo-14.4.01-decane was improved bv 6.2~; comnared to the system without ionic liauid.展开更多
文摘The synthesis of 1,4,5,8-tetramethoxynaphthalene-2-carboxaldehyde,an intermediate of shikonin was investigated.1,4,5,8-tetramethoxynaphthalene was prepared from the oxidation of 1,5-dinitronaphthalene and the reaction product naphthazarin was directly methylated without been purified.The title compound was obtained by the formylation of 1,4,5,8-tetramethoxynaphthalene.The overall yield was 38.5% based on 1,5-dinitronaphthalene.
基金Supported by the Youth Foundation of Nanyang Institute of Technology and Science&Technology Research Projects of Henan Provincial Education Department(14B150035)
文摘A novel coordination polymer [Ba2(AQTC)(H2O)3]n(1, H4 AQTC = anthraquinone-1,4,5,8-tetracarboxylic acid) has been prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectroscopy and thermogravimetric analysis. Two quinone oxygen atoms and all carboxylate oxygen atoms of AQTC4- are involved in coordination. Two equivalent barium ions are mainly linked by carboxylate oxygen atoms into a dimer. Neighbouring dimers are further connected by the AQTC4- ligand through carboxylate oxygen atom, leading to a 1-D chain structure. Every two adjacent chains are mainly further connected by face carboxylate oxygen atoms and water molecule, generating a two-dimensional layer structure. Such 2-D layer structures are connected with O(6) and O(6C) atoms from water molecules to form a 3-D structure. In addition, luminescent properties of 1 are also investigated.
基金financial support from the Nature Science Foundation of Jiangsu Province (No. BK2011697)
文摘An experimental study was carried out on the direct nitration of 1,4,5,8-tetraaza-bicyclo-[4,4,0]-decane to synthesize 1,4,5,8-tetranitro-l,4,5,8-tetraazabicyclo-[4,4,0]-decane (TNAD) with N205 catalyzed by acidic ionic liquids. Various ionic liquids, such as [HMim]X, [(CH2)4SO3HMim]X and [Capl]X (X =pTSO-, NO3 , HS04-), and various parameters such as equivalents of ionic liquid, molar ratio of N205 tO the starting material, reaction time and temperature, and solvent were investigated, Ionic liquid [(CH2)4SO3HMim]HS04 showed better catalytic activity. In the presence of 3% molar ratio of [(CH2)4SO3HMim]HS04 ionic liquid to the staring material, the yield of 1,4,5,8-tetranitro-l,4,5,8- tetraazabicvclo-14.4.01-decane was improved bv 6.2~; comnared to the system without ionic liauid.