Reaction of copper powder, dibenzoyl peroxide and 2-amino-4methyl-5-ethoxycarbonyl thiazole (amet) by refluxing in acetone yielded the dinuclearcopper(Ⅱ) complex Cu2 (μ-PhCOO)4 (amet)2- 2CH3COCH3. Crystal structure ...Reaction of copper powder, dibenzoyl peroxide and 2-amino-4methyl-5-ethoxycarbonyl thiazole (amet) by refluxing in acetone yielded the dinuclearcopper(Ⅱ) complex Cu2 (μ-PhCOO)4 (amet)2- 2CH3COCH3. Crystal structure determination showed that each copper atom is coordinated by four bridged benzoxy and oneamet molecule with an M-M bond (Cu-Cu (A) = 2.6899 (7 ) ), therefore the coor-dination environment around the copper center is a distorted square pyramid with N(1)at the apical position. Blocks of Cu2 (μ-PhCOO)4 (amet)2·2CH3COCH3 crystallize inthe triclinic space group Ph, with Mr= 1100.14, a= 9. 631 (1), b=10. 446 (2), c=12. 758(2) ; a=91. 31 (1), β=95. 50(1),γ= 94. 87(1)°, V=1272. 4(3), Z=1, Dc= 1. 436 g/cm3, F(000) = 570, μ=0. 986 mm-1 and R=0.033, Rw=0.049.The IR spectra, which are of great interest since the molecule has ketone, ester andcarboxylate group simultaneously, are also discussed.展开更多
An efficient three-component synthesis of 6-amino-4-aryl-5-cyano-3-metriyl-1-phenyl-1,4-dihydropyrano[2,3-c]pyrazoles via a reaction between 3-methyl-1-phenyl-2-pyrazolin-5-one,aromatic aldehydes and malononitrile usi...An efficient three-component synthesis of 6-amino-4-aryl-5-cyano-3-metriyl-1-phenyl-1,4-dihydropyrano[2,3-c]pyrazoles via a reaction between 3-methyl-1-phenyl-2-pyrazolin-5-one,aromatic aldehydes and malononitrile using tungstate sulfuric acid as a catalyst was described.Mild conditions,good to excellent yields,easily available catalyst and easy work-up are the key features of this method.展开更多
<span style="font-family:Verdana;">The present work describes the synthesis of a novel heterocyclic azo dye by </span><span style="font-family:Verdana;">general diazonization of 2...<span style="font-family:Verdana;">The present work describes the synthesis of a novel heterocyclic azo dye by </span><span style="font-family:Verdana;">general diazonization of 2-amino-4,5-dimethylthiazole followed by the di</span><span style="font-family:Verdana;">azo-</span><span><span><span style="font-family:;" "=""> </span></span></span><span><span><span style="font-family:;" "=""><span style="font-family:Verdana;">coupling of the resulting diazonium ion with 5-methyl-2-(propan-2-</span><span><span style="font-family:Verdana;">yl)phenol to obtain ligand </span><b><span style="font-family:Verdana;">L</span></b><span style="font-family:Verdana;">. This was characterized using Fouri</span></span><span style="font-family:Verdana;">er-transformed infrared and electronic spectrophotometry. Ligand </span><b><span style="font-family:Verdana;">L </span></b><span style="font-family:Verdana;">was further coordinated with five </span><span style="font-family:Verdana;">metal ions, M:L, 1:2 </span></span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">[</span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">M</span></span></span><span><span><span style="font-family:;" "=""> </span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">= Cu(II), Mn(II), Zn(II), Ni(II) and Co(II)</span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">]</span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">. The </span></span></span><span><span><span style="font-family:;" "=""><span style="font-family:Verdana;">coordination compounds obtained were characterized by electronic, IR spectrophotometry, magnetic susceptibility and percentage metal analyses. The results obtained suggested that a thiazoylazo dye was obtained as ligand </span><b><span style="font-family:Verdana;">L</span></b><span style="font-family:Verdana;">. It was proposed that two molecules of the solvent coordinated to the metal ion in addition with the ligands to give an octahedral geometry for copper(II), manganese(II) and nickel(II) complexes. On the other hand, square planar </span><span style="font-family:Verdana;">geometry was suggested for zinc(II) and cobalt(II) complexes. The an</span><span style="font-family:Verdana;">ti-infla</span></span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">- </span></span></span><span><span><span style="font-family:;" "=""><span style="font-family:Verdana;">mmatory activity of the ligand and coordination compounds was evaluated using four </span><i><span style="font-family:Verdana;">in</span></i> <i><span style="font-family:Verdana;">vitro</span></i><span style="font-family:Verdana;">-based assays viz: </span><span><span style="font-family:Verdana;">xanthine oxidase and lipoxygenase inhibition assay, membrane stability and protein denaturation assay. The synthesized compounds generally exhibited good anti-inflammatory activity in all </span><span style="font-family:Verdana;">the assays carried out. However, the reference standards, in this instance,</span><span style="font-family:Verdana;"> were more effective in the case of xanthine oxidase, lipoxygenase and protein denaturation inhibitory assays. For the membrane stability study, the </span><span><span style="font-family:Verdana;">coordination compounds and ligand </span><b><span style="font-family:Verdana;">L </span></b><span style="font-family:Verdana;">elicited more potent anti-inflammatory</span></span><span style="font-family:Verdana;"> activity than the standard drug.</span></span></span></span></span>展开更多
文摘Reaction of copper powder, dibenzoyl peroxide and 2-amino-4methyl-5-ethoxycarbonyl thiazole (amet) by refluxing in acetone yielded the dinuclearcopper(Ⅱ) complex Cu2 (μ-PhCOO)4 (amet)2- 2CH3COCH3. Crystal structure determination showed that each copper atom is coordinated by four bridged benzoxy and oneamet molecule with an M-M bond (Cu-Cu (A) = 2.6899 (7 ) ), therefore the coor-dination environment around the copper center is a distorted square pyramid with N(1)at the apical position. Blocks of Cu2 (μ-PhCOO)4 (amet)2·2CH3COCH3 crystallize inthe triclinic space group Ph, with Mr= 1100.14, a= 9. 631 (1), b=10. 446 (2), c=12. 758(2) ; a=91. 31 (1), β=95. 50(1),γ= 94. 87(1)°, V=1272. 4(3), Z=1, Dc= 1. 436 g/cm3, F(000) = 570, μ=0. 986 mm-1 and R=0.033, Rw=0.049.The IR spectra, which are of great interest since the molecule has ketone, ester andcarboxylate group simultaneously, are also discussed.
文摘An efficient three-component synthesis of 6-amino-4-aryl-5-cyano-3-metriyl-1-phenyl-1,4-dihydropyrano[2,3-c]pyrazoles via a reaction between 3-methyl-1-phenyl-2-pyrazolin-5-one,aromatic aldehydes and malononitrile using tungstate sulfuric acid as a catalyst was described.Mild conditions,good to excellent yields,easily available catalyst and easy work-up are the key features of this method.
文摘<span style="font-family:Verdana;">The present work describes the synthesis of a novel heterocyclic azo dye by </span><span style="font-family:Verdana;">general diazonization of 2-amino-4,5-dimethylthiazole followed by the di</span><span style="font-family:Verdana;">azo-</span><span><span><span style="font-family:;" "=""> </span></span></span><span><span><span style="font-family:;" "=""><span style="font-family:Verdana;">coupling of the resulting diazonium ion with 5-methyl-2-(propan-2-</span><span><span style="font-family:Verdana;">yl)phenol to obtain ligand </span><b><span style="font-family:Verdana;">L</span></b><span style="font-family:Verdana;">. This was characterized using Fouri</span></span><span style="font-family:Verdana;">er-transformed infrared and electronic spectrophotometry. Ligand </span><b><span style="font-family:Verdana;">L </span></b><span style="font-family:Verdana;">was further coordinated with five </span><span style="font-family:Verdana;">metal ions, M:L, 1:2 </span></span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">[</span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">M</span></span></span><span><span><span style="font-family:;" "=""> </span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">= Cu(II), Mn(II), Zn(II), Ni(II) and Co(II)</span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">]</span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">. The </span></span></span><span><span><span style="font-family:;" "=""><span style="font-family:Verdana;">coordination compounds obtained were characterized by electronic, IR spectrophotometry, magnetic susceptibility and percentage metal analyses. The results obtained suggested that a thiazoylazo dye was obtained as ligand </span><b><span style="font-family:Verdana;">L</span></b><span style="font-family:Verdana;">. It was proposed that two molecules of the solvent coordinated to the metal ion in addition with the ligands to give an octahedral geometry for copper(II), manganese(II) and nickel(II) complexes. On the other hand, square planar </span><span style="font-family:Verdana;">geometry was suggested for zinc(II) and cobalt(II) complexes. The an</span><span style="font-family:Verdana;">ti-infla</span></span></span></span><span style="font-family:Verdana;"><span style="font-family:Verdana;"><span style="font-family:Verdana;">- </span></span></span><span><span><span style="font-family:;" "=""><span style="font-family:Verdana;">mmatory activity of the ligand and coordination compounds was evaluated using four </span><i><span style="font-family:Verdana;">in</span></i> <i><span style="font-family:Verdana;">vitro</span></i><span style="font-family:Verdana;">-based assays viz: </span><span><span style="font-family:Verdana;">xanthine oxidase and lipoxygenase inhibition assay, membrane stability and protein denaturation assay. The synthesized compounds generally exhibited good anti-inflammatory activity in all </span><span style="font-family:Verdana;">the assays carried out. However, the reference standards, in this instance,</span><span style="font-family:Verdana;"> were more effective in the case of xanthine oxidase, lipoxygenase and protein denaturation inhibitory assays. For the membrane stability study, the </span><span><span style="font-family:Verdana;">coordination compounds and ligand </span><b><span style="font-family:Verdana;">L </span></b><span style="font-family:Verdana;">elicited more potent anti-inflammatory</span></span><span style="font-family:Verdana;"> activity than the standard drug.</span></span></span></span></span>