Action of bromine in concentrated nitric acid allows carrying out mono- and polybromination of moderately deactivated aromatic compounds. 4-Chloronitrobenzene and isophthalic acid turnes into 3-bromo-4-chloronitrobenz...Action of bromine in concentrated nitric acid allows carrying out mono- and polybromination of moderately deactivated aromatic compounds. 4-Chloronitrobenzene and isophthalic acid turnes into 3-bromo-4-chloronitrobenzene and 5-bromoisophthalic acid at reaction with bromine in concentrated nitric acid at 20°C whereas in absence of bromine in the same conditions 4-chloro-1, 3-dinitrobenzene and 5-nitroisophthalic acid are formed accordingly. Presence of bromine in concentrated nitric acid changes nitrating capacity to brominating one. Terephthalic acid and phthalic anhydride at heating with bromine in concentrated nitric acid can be transformed to appropriating tetrabromo substituted compounds.展开更多
Two 2D layer complexes {[La（TBTA）1.5（phen）2H2O].3H2O}n （1） and {[Ce（TBTA）l.5（phen）2H2O]-3H2O}n （2） （H2TBTA = 2,3,5,6-tetrabromoterephthalic acid, phen = 1.10-phenanthroline） have been synthesized and cha...Two 2D layer complexes {[La（TBTA）1.5（phen）2H2O].3H2O}n （1） and {[Ce（TBTA）l.5（phen）2H2O]-3H2O}n （2） （H2TBTA = 2,3,5,6-tetrabromoterephthalic acid, phen = 1.10-phenanthroline） have been synthesized and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectra and thermogravimetric analyses. Both crystals belong to monoclinic, space group P21/n. Crystal data for 1： a = 8.7097（11）, b = 34.276（4）, c = 13.7281（17） A, β = 95.397（2）°, V= 4080.1（9） A3, Z = 4, LaC36H24Br6N4O10, Mr= 1290.96, Dc = 2.102 g/cm3,μ（MoKa） = 6.983 mm-1, F（000） = 2460.0, T = 296（2） K, the final R （I 〉 2σ（I）） = 0.0478 and wR （all data） = 0.0985 for 10127 independent （Rint = 0.0775） and 7137 observed reflections with I 〉 2σ（I）. Crystal data for 2： a = 8.709（2）, b = 34.202（9）, c = 13.685（4） A, β = 95.714（4）, V= 4055.9（19） A3, Z = 4, CeBr6C36H24O10N4, Mr = 1292.17, Dc = 2.116 g/cm3, μ（MoKa） = 7.094 mm-1, F（000） = 2464.0, T= 296（2） K, the final R（I 〉 2σ（I）） = 0.0590 and wR（all data） = 0.1453 for 10014 independent （Rint = 0.1253） and 6081 observed reflections with I 〉 2σ（I）. Both complexes are allomerism with the general molecular formula of {[M（TBTA）1.5（phen）2H2O].3H2O}n. In the structures, the H2TBTA ligands adopt a monodentate coordination mode. Both the 2D layer frameworks are further extended to be 3D layers via H-bonding interactions.展开更多
The complex [Tm（TBTA）1.5（bipy）（H2O）2]n （H2TBTA = 2,3,5,6-tetrabromoterephthalic acid, bipy = 2,2-bipyridyl） has been synthesized in water-methanol solution at ambient temperature and characterized by single-cr...The complex [Tm（TBTA）1.5（bipy）（H2O）2]n （H2TBTA = 2,3,5,6-tetrabromoterephthalic acid, bipy = 2,2-bipyridyl） has been synthesized in water-methanol solution at ambient temperature and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum and thermogravimetric analysis. The crystal belongs to triclinic, space group P1 with a = 11.1429（2）, b = 11.485（2）, c = 12.872（2）, V = 1498.1（5）3 , Z = 2, C22H14Br6N2O9Tm, Mr = 1098.74, Dc = 2.436 g/cm3 , μ（MoKα） = 11.013 mm-1 , F（000） = 1022, T = 296.15 K, the final R （I 〉2σ（I）） = 0.0494 and wR （all data） = 0.1246. The asymmetric unit of the complex is composed of one Tm ion, one and a half of coordinated TBTA 2-anions, one bipy, two coordinated and one lattice water molecules. The adjacent metal ions are bridged by TBTA 2- anions to form a 2D wave-like layer.展开更多
文摘Action of bromine in concentrated nitric acid allows carrying out mono- and polybromination of moderately deactivated aromatic compounds. 4-Chloronitrobenzene and isophthalic acid turnes into 3-bromo-4-chloronitrobenzene and 5-bromoisophthalic acid at reaction with bromine in concentrated nitric acid at 20°C whereas in absence of bromine in the same conditions 4-chloro-1, 3-dinitrobenzene and 5-nitroisophthalic acid are formed accordingly. Presence of bromine in concentrated nitric acid changes nitrating capacity to brominating one. Terephthalic acid and phthalic anhydride at heating with bromine in concentrated nitric acid can be transformed to appropriating tetrabromo substituted compounds.
基金Supported by the International Scientific and Technological Cooperation Projects of Shanxi Province (2011081022)International S&T Cooperation Program of China (No. 2011DFA51980)the Natural Science Foundation of Shanxi Province (No. 2009021024)
文摘Two 2D layer complexes {[La（TBTA）1.5（phen）2H2O].3H2O}n （1） and {[Ce（TBTA）l.5（phen）2H2O]-3H2O}n （2） （H2TBTA = 2,3,5,6-tetrabromoterephthalic acid, phen = 1.10-phenanthroline） have been synthesized and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectra and thermogravimetric analyses. Both crystals belong to monoclinic, space group P21/n. Crystal data for 1： a = 8.7097（11）, b = 34.276（4）, c = 13.7281（17） A, β = 95.397（2）°, V= 4080.1（9） A3, Z = 4, LaC36H24Br6N4O10, Mr= 1290.96, Dc = 2.102 g/cm3,μ（MoKa） = 6.983 mm-1, F（000） = 2460.0, T = 296（2） K, the final R （I 〉 2σ（I）） = 0.0478 and wR （all data） = 0.0985 for 10127 independent （Rint = 0.0775） and 7137 observed reflections with I 〉 2σ（I）. Crystal data for 2： a = 8.709（2）, b = 34.202（9）, c = 13.685（4） A, β = 95.714（4）, V= 4055.9（19） A3, Z = 4, CeBr6C36H24O10N4, Mr = 1292.17, Dc = 2.116 g/cm3, μ（MoKa） = 7.094 mm-1, F（000） = 2464.0, T= 296（2） K, the final R（I 〉 2σ（I）） = 0.0590 and wR（all data） = 0.1453 for 10014 independent （Rint = 0.1253） and 6081 observed reflections with I 〉 2σ（I）. Both complexes are allomerism with the general molecular formula of {[M（TBTA）1.5（phen）2H2O].3H2O}n. In the structures, the H2TBTA ligands adopt a monodentate coordination mode. Both the 2D layer frameworks are further extended to be 3D layers via H-bonding interactions.
基金Supported by the International Scientific and Technological Cooperation Projects of Shanxi Province (2011081022)International S&T Cooperation Program of China (2011DFA51980)
文摘The complex [Tm（TBTA）1.5（bipy）（H2O）2]n （H2TBTA = 2,3,5,6-tetrabromoterephthalic acid, bipy = 2,2-bipyridyl） has been synthesized in water-methanol solution at ambient temperature and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum and thermogravimetric analysis. The crystal belongs to triclinic, space group P1 with a = 11.1429（2）, b = 11.485（2）, c = 12.872（2）, V = 1498.1（5）3 , Z = 2, C22H14Br6N2O9Tm, Mr = 1098.74, Dc = 2.436 g/cm3 , μ（MoKα） = 11.013 mm-1 , F（000） = 1022, T = 296.15 K, the final R （I 〉2σ（I）） = 0.0494 and wR （all data） = 0.1246. The asymmetric unit of the complex is composed of one Tm ion, one and a half of coordinated TBTA 2-anions, one bipy, two coordinated and one lattice water molecules. The adjacent metal ions are bridged by TBTA 2- anions to form a 2D wave-like layer.
