Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). Th...Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.展开更多
A new 3D supramolecular complex,namely dimethylammonium 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoate)dihydrate,has been synthesized by the reaction of 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenz...A new 3D supramolecular complex,namely dimethylammonium 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoate)dihydrate,has been synthesized by the reaction of 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoic acid)with aqueous dimethylamine solution and characterized by single-crystal X-ray diffraction,^(1)H NMR spectroscopy and elemental analysis.It belongs to triclinic system,space groupP with a=6.5539(4),b=9.4977(6),c=12.1407(8)Å,α=72.299(6),β=89.160(5),γ=70.797(8)°,V=676.52(8)Å^(3),Z=1,Mr=556.57,µ=0.103 mm^(-1),Dc=1.366 g/cm^(3),F(000)=294,the final R=0.0828 and wR=0.2083 for 1934 observed reflections with I>2σ(I).The 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoic acid)dianion,dimethylammonium cation,and water molecule are interconnected by O−H∙∙∙O,N−H∙∙∙N,and N−H∙∙∙O hydrogen bonds,forming a two-dimensional(2D)layer.Two adjacent 2D layers are further stacked into a three-dimensional supramolecular structure through O−H∙∙∙O hydrogen bonds.In addition,the luminescent property of this supramolecular complex has also been investigated.展开更多
文摘Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.
基金the National Natural Science Foundation of China(21372112)。
文摘A new 3D supramolecular complex,namely dimethylammonium 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoate)dihydrate,has been synthesized by the reaction of 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoic acid)with aqueous dimethylamine solution and characterized by single-crystal X-ray diffraction,^(1)H NMR spectroscopy and elemental analysis.It belongs to triclinic system,space groupP with a=6.5539(4),b=9.4977(6),c=12.1407(8)Å,α=72.299(6),β=89.160(5),γ=70.797(8)°,V=676.52(8)Å^(3),Z=1,Mr=556.57,µ=0.103 mm^(-1),Dc=1.366 g/cm^(3),F(000)=294,the final R=0.0828 and wR=0.2083 for 1934 observed reflections with I>2σ(I).The 4,4΄-([2,2΄-bipyrimidine]-5,5΄-diyl)bis(2-hydroxybenzoic acid)dianion,dimethylammonium cation,and water molecule are interconnected by O−H∙∙∙O,N−H∙∙∙N,and N−H∙∙∙O hydrogen bonds,forming a two-dimensional(2D)layer.Two adjacent 2D layers are further stacked into a three-dimensional supramolecular structure through O−H∙∙∙O hydrogen bonds.In addition,the luminescent property of this supramolecular complex has also been investigated.
