Synthetic method of asymmetry polyarylamino\|benzaldehydes by the selective formylation of polyarylamines in Vilsmeier\|Haack reaction was studied. Five polyarylamino\|benzaldehydes, \{4\|\%N\|\%methylphenylamino\}\|b...Synthetic method of asymmetry polyarylamino\|benzaldehydes by the selective formylation of polyarylamines in Vilsmeier\|Haack reaction was studied. Five polyarylamino\|benzaldehydes, \{4\|\%N\|\%methylphenylamino\}\|benzaldehyde, 4\|\%N\|\%（\%n\%\|butyl）\|phenylamino\|benzaldehyde, 4\|diphenylamino\|benzaldehyde, 4\|\%N\|\%phenyl\|diphenylamino\|benzaldehyde, 4\|\%N\|\%phenyl\|（4′\|diphenylamino）diphenylamino\|benzaldehyde were synthesized by the selective formylation of the polyarylamines with POCl\-3 and DMF in the yields of 67%\92%. The structures of these aldehydes were characterized by MS, \{\}\+1H NMR, IR. The studied results showed that the yields and selectivity of asymmetry polyarylamino\|benzaldehydes were found to relate with the reaction time, structures of polyarylamines and the molar ratio of the reactants.展开更多
The crystal structures of fluoride and chloride complexes of tris[（2-benzimidazolyl）methyl]amine 1 were characterized by X-ray crystallography. 1 adopts （73 symmetrical geometry and cone-like conformation so as to ...The crystal structures of fluoride and chloride complexes of tris[（2-benzimidazolyl）methyl]amine 1 were characterized by X-ray crystallography. 1 adopts （73 symmetrical geometry and cone-like conformation so as to allow its three NHs to associate with the anions through hydrogen bonds. Despite the different sizes of the anions, the two crystals are unexpectedly isostructural. The binding ability of the anions of 1 in solution was also studied by using of UV-vis spectroscopy.展开更多
3,3＇-Bis（5-（N-（4-hydroxylphenyl）imidomethyl）pyrrol-2-yl）pentane 1 has been synthesized and characterized. The crystal of its methanol complex, 1·（CH3OH）2, belongs to the orthorhombic system, space group ...3,3＇-Bis（5-（N-（4-hydroxylphenyl）imidomethyl）pyrrol-2-yl）pentane 1 has been synthesized and characterized. The crystal of its methanol complex, 1·（CH3OH）2, belongs to the orthorhombic system, space group Pccn with a = 18.094（2）, b = 11.6890（16）, c = 13.3629（19） , V = 2826.3（7） 3, Z = 8, C14.5H18N2O2, Mr = 252.31, Dc = 1.186 g/cm3, F（000） = 1080 and μ（MoKα） = 0.080 mm-1. The final R = 0.0662 and wR = 0.1801 for 1908 observed reflections with I 2σ（I）, and R = 0.0800 and wR = 0.1948 for all reflections. In the solid state, bridged by included methanol molecules, the molecules of compound 1 form interpenetrated grid structure through N–H···O and O–H···O hydrogen bonds.展开更多
The reactions of 5,5＇-bis（2-acylphenyl）diazo-dipyrromethane （H2L） with CuSO4 and NiCl2 resulted in the formation of corresponding mononuclear coordination complexes 2 （CuL） and 3 （NIL）. The crystal of complex...The reactions of 5,5＇-bis（2-acylphenyl）diazo-dipyrromethane （H2L） with CuSO4 and NiCl2 resulted in the formation of corresponding mononuclear coordination complexes 2 （CuL） and 3 （NIL）. The crystal of complex 2 is of monoclinic system, space group P21 with a = 10.040（5）, b = 11.900（5）, c = 11.170（5） A, β = 93.057（8）°, V = 1332.8（2） A3, Z = 2, C29H28N602Cu, Mr = 556.11, Dc = 1.386 g/cm, F（000） = 578 and/z（MoKa） = 0.857 mm^-1. The crystal of complex 3 belongs to the monoclinic system, space group P21/n with a = 12.0445（6）, b = 17.2101（8）, c = 16.3304（6） A, β = 128.407（2）°, V = 2654.6（2） A3, Z = 4, C29H28N6O2Ni, Mr= 551.28, Dc= 1.380 g/cm, F（000） = 1152 and μ（MoKa） = 0.770 mm^-1. In both complexes, the metal ions are in square-planar geometry by coordinating to two azo N atoms and two deprotonated pyrrole N atoms. Intramolecular Cu…O=C in complex 2 and intermolecular Ni…O=C in complex 3 were found. The UV-Vis spectra and thermal stability of complexes 2 and 3 were also studied.展开更多
A new 5,5＇-bisdiazo dipyrromethane, compound 2, has been synthesized and cha- racterized. The crystal of 2 is of monoclinic, space group P21/c with a = 16.3185（10）, b = 20.8225（13）, c = 18.5985（11） ）k, β = 11...A new 5,5＇-bisdiazo dipyrromethane, compound 2, has been synthesized and cha- racterized. The crystal of 2 is of monoclinic, space group P21/c with a = 16.3185（10）, b = 20.8225（13）, c = 18.5985（11） ）k, β = 114.5280（10）°, V = 5749.3（6） ）A^3, Z = 8, C25H26N602, Mr= 442.52, Dc= 1.022 g/cm, F（000） = 1872,/x（MoKa） = 0.068 mmI. The final R = 0.0469 and wR = 0.1143 for 10119 observed reflections with I 〉 2tr（/）, and R = 0.0677 and wR = 0.1231 for all reflections. The title compound prefers to form interlocked type dimer through quadruple N-H...N hydrogen bonds. The dimers self-assemble into a porous 3-D structure through O-H...O and C-H...N hydrogen bonds.展开更多
A new 5,5＇-bisdiazo-dipyrromethane compound 3 has been synthesized and cha- racterized. The crystal of 3 is of orthorhombic, space group Iba2 with a = 19.1914（17）, b = 9.8396（8）, c = 13.7643（12） A, V= 2599.2（4...A new 5,5＇-bisdiazo-dipyrromethane compound 3 has been synthesized and cha- racterized. The crystal of 3 is of orthorhombic, space group Iba2 with a = 19.1914（17）, b = 9.8396（8）, c = 13.7643（12） A, V= 2599.2（4） A3, Z = 4, C29H34N602, Mr = 498.62, Dc = 1.274 g/cm3, F（000） = 1064, μ（MoKa） = 0.083 mm-1, the final R = 0.0302 and wR = 0.0786 for 6361 observed reflections with I 〉 2σ（/）, and R = 0.0320 and wR = 0.08006 for all data. It reveals that the molecules of compound 3 assemble into grid structures through a R22（7） type hydrogen bonding motif between azopyrrole and hydroxyl group. The grids interpenetrate each other with the assistance of C-H...π interaction.展开更多
文摘Synthetic method of asymmetry polyarylamino\|benzaldehydes by the selective formylation of polyarylamines in Vilsmeier\|Haack reaction was studied. Five polyarylamino\|benzaldehydes, \{4\|\%N\|\%methylphenylamino\}\|benzaldehyde, 4\|\%N\|\%（\%n\%\|butyl）\|phenylamino\|benzaldehyde, 4\|diphenylamino\|benzaldehyde, 4\|\%N\|\%phenyl\|diphenylamino\|benzaldehyde, 4\|\%N\|\%phenyl\|（4′\|diphenylamino）diphenylamino\|benzaldehyde were synthesized by the selective formylation of the polyarylamines with POCl\-3 and DMF in the yields of 67%\92%. The structures of these aldehydes were characterized by MS, \{\}\+1H NMR, IR. The studied results showed that the yields and selectivity of asymmetry polyarylamino\|benzaldehydes were found to relate with the reaction time, structures of polyarylamines and the molar ratio of the reactants.
基金the National Natural Science Foundation of China (No. 20702038)the University Science Foundation of Tianjin Education Committee (20050609)Tianjin Normal University
文摘The crystal structures of fluoride and chloride complexes of tris[（2-benzimidazolyl）methyl]amine 1 were characterized by X-ray crystallography. 1 adopts （73 symmetrical geometry and cone-like conformation so as to allow its three NHs to associate with the anions through hydrogen bonds. Despite the different sizes of the anions, the two crystals are unexpectedly isostructural. The binding ability of the anions of 1 in solution was also studied by using of UV-vis spectroscopy.
基金supported by the National Natural Science Foundation of China (No. 20702038)
文摘3,3＇-Bis（5-（N-（4-hydroxylphenyl）imidomethyl）pyrrol-2-yl）pentane 1 has been synthesized and characterized. The crystal of its methanol complex, 1·（CH3OH）2, belongs to the orthorhombic system, space group Pccn with a = 18.094（2）, b = 11.6890（16）, c = 13.3629（19） , V = 2826.3（7） 3, Z = 8, C14.5H18N2O2, Mr = 252.31, Dc = 1.186 g/cm3, F（000） = 1080 and μ（MoKα） = 0.080 mm-1. The final R = 0.0662 and wR = 0.1801 for 1908 observed reflections with I 2σ（I）, and R = 0.0800 and wR = 0.1948 for all reflections. In the solid state, bridged by included methanol molecules, the molecules of compound 1 form interpenetrated grid structure through N–H···O and O–H···O hydrogen bonds.
基金supported by the National Natural Science Foundation of China(NSFC No.21172174)Program of Study Abroad for Young Scholar sponsored by Tianjin Municipal Education Commission
文摘The reactions of 5,5＇-bis（2-acylphenyl）diazo-dipyrromethane （H2L） with CuSO4 and NiCl2 resulted in the formation of corresponding mononuclear coordination complexes 2 （CuL） and 3 （NIL）. The crystal of complex 2 is of monoclinic system, space group P21 with a = 10.040（5）, b = 11.900（5）, c = 11.170（5） A, β = 93.057（8）°, V = 1332.8（2） A3, Z = 2, C29H28N602Cu, Mr = 556.11, Dc = 1.386 g/cm, F（000） = 578 and/z（MoKa） = 0.857 mm^-1. The crystal of complex 3 belongs to the monoclinic system, space group P21/n with a = 12.0445（6）, b = 17.2101（8）, c = 16.3304（6） A, β = 128.407（2）°, V = 2654.6（2） A3, Z = 4, C29H28N6O2Ni, Mr= 551.28, Dc= 1.380 g/cm, F（000） = 1152 and μ（MoKa） = 0.770 mm^-1. In both complexes, the metal ions are in square-planar geometry by coordinating to two azo N atoms and two deprotonated pyrrole N atoms. Intramolecular Cu…O=C in complex 2 and intermolecular Ni…O=C in complex 3 were found. The UV-Vis spectra and thermal stability of complexes 2 and 3 were also studied.
基金Supported by the NNSFC (No.21172174, 20702038)Innovation Foundation of Tianjin Normal University (52XC1101)
文摘A new 5,5＇-bisdiazo dipyrromethane, compound 2, has been synthesized and cha- racterized. The crystal of 2 is of monoclinic, space group P21/c with a = 16.3185（10）, b = 20.8225（13）, c = 18.5985（11） ）k, β = 114.5280（10）°, V = 5749.3（6） ）A^3, Z = 8, C25H26N602, Mr= 442.52, Dc= 1.022 g/cm, F（000） = 1872,/x（MoKa） = 0.068 mmI. The final R = 0.0469 and wR = 0.1143 for 10119 observed reflections with I 〉 2tr（/）, and R = 0.0677 and wR = 0.1231 for all reflections. The title compound prefers to form interlocked type dimer through quadruple N-H...N hydrogen bonds. The dimers self-assemble into a porous 3-D structure through O-H...O and C-H...N hydrogen bonds.
基金supported by the National Natural Science Foundation of China(NSFCNo.20702038,21172174)Innovation Foundation of Tianjin Normal University(52XC1101)
文摘A new 5,5＇-bisdiazo-dipyrromethane compound 3 has been synthesized and cha- racterized. The crystal of 3 is of orthorhombic, space group Iba2 with a = 19.1914（17）, b = 9.8396（8）, c = 13.7643（12） A, V= 2599.2（4） A3, Z = 4, C29H34N602, Mr = 498.62, Dc = 1.274 g/cm3, F（000） = 1064, μ（MoKa） = 0.083 mm-1, the final R = 0.0302 and wR = 0.0786 for 6361 observed reflections with I 〉 2σ（/）, and R = 0.0320 and wR = 0.08006 for all data. It reveals that the molecules of compound 3 assemble into grid structures through a R22（7） type hydrogen bonding motif between azopyrrole and hydroxyl group. The grids interpenetrate each other with the assistance of C-H...π interaction.
