Two series of solid complexes of europium and terbium with biphenyl 4-carboxylic acid and phen were synthesized and characterized in this report. Their elemental analysis, molar conductivities and TG-DTA studies indic...Two series of solid complexes of europium and terbium with biphenyl 4-carboxylic acid and phen were synthesized and characterized in this report. Their elemental analysis, molar conductivities and TG-DTA studies indicate that the complexes have the composition of Eu(phen)L3·1/2H2O, Eu0.5RE0.5(phen) L3·1/2H2O; Tb (phen) L3·H2O and Tb0.5 RE0.5(Phen)L3·1/2H2O. (RE = Y3+, La3+ and Gd3+; L = biphenyl 4-carboxylic acid; phen = o-Phenanthroline). The studies of their IR, UV 1H NMR and molar conductivities demonstrate that biphenyl 4-carboylic acid is bounded with RE (III ) ion. Rare earth ions coordinate with two nitrogen atoms of phen molecules directly in these rare earth complexes. The fluorescence spectra and fluorescence lifetimes of the rare earth complexes show that the fluorescent intensity and lifetime of a series of europium complexes are longer than those of the series of terbium complexes as having the some ligands. There are better fluorescent intensity and lifetime of hetero-nuclear rare earth complexes than homo-nuclear rare earth complexes for europium complexes. The fluorescence emission intensity of Eu3 + is raised by inert fluorescent rare earth ions (Y3+ , Gd3+ and La3+ ), but in Tb3+ hetero-nuclear rare earth complexes the intensity of Tb3+ ions are quenched by the inert fluorescent rare earth ions.展开更多
A novel cobalt complex,[Co2(bptc)(bix)1.5](1,H4bptc=3,3',4,4'-biphenyltetra-carboxylic acid,bix = 1,4-bis(imidazol-1-ylmethyl)benzene),has been hydrothermally prepared and characterized by IR spectroscopy,el...A novel cobalt complex,[Co2(bptc)(bix)1.5](1,H4bptc=3,3',4,4'-biphenyltetra-carboxylic acid,bix = 1,4-bis(imidazol-1-ylmethyl)benzene),has been hydrothermally prepared and characterized by IR spectroscopy,elemental analysis and single-crystal X-ray diffraction.The crystal is of triclinic system,space group P1 with a=10.770(7),b=12.245(8),c=13.514(9),α=102.829(8),β=107.734(8),γ=98.833(9)°,C37H27N6O8Co2,Mr=801.51,V=1607.5(18)3,Dc=1.656g/cm3,F(000)=818,μ=1.100mm-1,Z=2,the final R = 0.0694 and wR = 0.1543 for 3034 observed reflections(I2σ(I)).In the title complex,the two Co(Ⅱ) ions are in different coordination environments with distorted octahedral and trigonal bipyramidal geometries,respectively.The Co atoms are linked together through hexadentate bptc ligands,giving rise to 2D layers which are bridged by the bix ligands into a 3-D supramolecular network.Magnetic susceptibilities of 1 reveal weak antiferromagnetic exchange interactions between the adjacent Co(Ⅱ) ions.展开更多
The title compound C18H16N4O3 (Mr = 336.35) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expect...The title compound C18H16N4O3 (Mr = 336.35) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632(1), b = 7.816(1), c = 28.082(5) A,β = 96.18(1)°, V= 1665.48(51) A^3, Z= 4, Dc = 1.341 g/cm^3, F(000) = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C(11)-C(16) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0.03 A) with the dihedral angle between them of 9.8%.展开更多
The effect of UV irradiation and blending with phthalate and terephthalate plasticizers on the photo-stability of Poly (4-vinyl biphenyl) was studied at different intervals of irradiation time and in presence of air. ...The effect of UV irradiation and blending with phthalate and terephthalate plasticizers on the photo-stability of Poly (4-vinyl biphenyl) was studied at different intervals of irradiation time and in presence of air. The increase in irradiation time on the photodegradation of polymer thin films caused a change in the intensity and shape of the fluorescence band. It has been found that the stability of the polymer decreases with the increase of irradiation time, and to increases with the increase of the amount of added phthalate and terephthalate plasticizers, which is evidence of polymer photodegradation. The FT-IR spectra of irradiated pure and blended polymer with phthalate and terephthalate plasticizers showed a decrease in some absorption bands and increase in the other bands, this is also another factor for the occurrence of photo degradation of the irradiated polymer. The increase in the intensity of absorption of carbonyl and hydroxyl region, indicates a possible photogegradation of polymeric chains and the formation of alcohols, aliphatic ketones and to the increase in the number of (C=C) that resulted from hydrogen abstraction during chains-scission.展开更多
Novel fluorine substituted α-amino phosphonic acids containing 1,2,4-triazin- 5-one (6a-f) have been obtained from fluoroacylation of 6-(2′-amino-5′-nitrophenyl)-3-thioxo-1,2,4-triazin-5(4H)-one (...Novel fluorine substituted α-amino phosphonic acids containing 1,2,4-triazin- 5-one (6a-f) have been obtained from fluoroacylation of 6-(2′-amino-5′-nitrophenyl)-3-thioxo-1,2,4-triazin-5(4H)-one (1) followed by ammonilysis to give the corresponding 3-amino-derivative 3. Condensation of compound 3 with nitro/halogenated aromatic aldehydes yielded the Schiff bases 4. The simple addition of diethyl phosphonate to compound 4 produced the α-amino phosphonates 5. Acidic hydrolysis of compound 5 produced the fluorine substituted α-amino acids derivatives 6. Structures of the new compounds have been established with the help of elemental analysis and spectral measurements. Also, the products evaluated as antioxidants, where the fluorinated α-amino phosphonic acids 6 are more active than the other synthesized systems.展开更多
Eighteen 2′,4′-difluoro-3-(carbamoyl)biphenyl-4-yl benzoates were synthesized from diflunisal in three steps with total yields from 72% to 86%. All compounds were identified by IR, 1^H NMR, MS and elemental analys...Eighteen 2′,4′-difluoro-3-(carbamoyl)biphenyl-4-yl benzoates were synthesized from diflunisal in three steps with total yields from 72% to 86%. All compounds were identified by IR, 1^H NMR, MS and elemental analysis. The anti-inflammatory activity and analgesic activity for 18 compounds were evaluated. The preliminary assay results showed that compounds 4a and 4p exhibited potent anti-inflammatory-analgesic activity.展开更多
The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ f...The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356(2), b = 7.0761(11), c = 20.539(3) A, β = 105.723(4)°, V= 1868.5(5) A3 and Z = 4.展开更多
The title compound (C16H15N3O2, Mr= 281.31) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expect...The title compound (C16H15N3O2, Mr= 281.31) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the C=N double bond. It crystallizes in the monoclinic system, space group P2 1/c with a = 11.150(3), b = 9.906(3), c = 13.624(4) A, β = 106.360(4)°, V= 1443.9(7) ,A^3, Z = 4, Dc = 1.294 g/cm^3, F(000) = 592,μ(MoKa) = 0.088 mm ^-1, R = 0.0577 and wR = 0.1214. Of the 5766 total reflections, 2540 were unique. In the molecule there exist two different planes of pyrazoline and O(2)-C(10) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0026 A) with the dihedral angle between them of 6.3°.展开更多
A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA...A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA), 4, 4'-biphenyl-bis-[4-phthalazin-1(2H)-one], 4, 4- difluorodiphenylketone (DFK). The monomer and copolymer were characterized by FT-IR and 1H-NMR. DSC and TGA were used to the novel polymer.展开更多
Six N-alkyl-4'-methyl-1,1'-biphenyl-2-sulfonamides were synthesized facilely and efficiently from low cost and readily available benzenesulfonyl chloride and C1-C4 fatty amines via linking DoM reaction with Suzuki r...Six N-alkyl-4'-methyl-1,1'-biphenyl-2-sulfonamides were synthesized facilely and efficiently from low cost and readily available benzenesulfonyl chloride and C1-C4 fatty amines via linking DoM reaction with Suzuki reaction.The structures of the new compounds synthesized were confirmed by elemental analysis,IR,1H NMR and MS.This new method makes a feature of low cost and readily available starting material,fewer steps,mild condition,easiness to operate and higher yield.展开更多
基金Project supported by the National Natural Science Foundation of China (20461002)Chunhui Plan of MOE (Z2004-2-15029)
文摘Two series of solid complexes of europium and terbium with biphenyl 4-carboxylic acid and phen were synthesized and characterized in this report. Their elemental analysis, molar conductivities and TG-DTA studies indicate that the complexes have the composition of Eu(phen)L3·1/2H2O, Eu0.5RE0.5(phen) L3·1/2H2O; Tb (phen) L3·H2O and Tb0.5 RE0.5(Phen)L3·1/2H2O. (RE = Y3+, La3+ and Gd3+; L = biphenyl 4-carboxylic acid; phen = o-Phenanthroline). The studies of their IR, UV 1H NMR and molar conductivities demonstrate that biphenyl 4-carboylic acid is bounded with RE (III ) ion. Rare earth ions coordinate with two nitrogen atoms of phen molecules directly in these rare earth complexes. The fluorescence spectra and fluorescence lifetimes of the rare earth complexes show that the fluorescent intensity and lifetime of a series of europium complexes are longer than those of the series of terbium complexes as having the some ligands. There are better fluorescent intensity and lifetime of hetero-nuclear rare earth complexes than homo-nuclear rare earth complexes for europium complexes. The fluorescence emission intensity of Eu3 + is raised by inert fluorescent rare earth ions (Y3+ , Gd3+ and La3+ ), but in Tb3+ hetero-nuclear rare earth complexes the intensity of Tb3+ ions are quenched by the inert fluorescent rare earth ions.
基金supported by the National Natural Science Foundation of China (No 20971004)the Outstanding Youth Foundation of Education Commission of Anhui Province (No 2010SQRL108ZD)
文摘A novel cobalt complex,[Co2(bptc)(bix)1.5](1,H4bptc=3,3',4,4'-biphenyltetra-carboxylic acid,bix = 1,4-bis(imidazol-1-ylmethyl)benzene),has been hydrothermally prepared and characterized by IR spectroscopy,elemental analysis and single-crystal X-ray diffraction.The crystal is of triclinic system,space group P1 with a=10.770(7),b=12.245(8),c=13.514(9),α=102.829(8),β=107.734(8),γ=98.833(9)°,C37H27N6O8Co2,Mr=801.51,V=1607.5(18)3,Dc=1.656g/cm3,F(000)=818,μ=1.100mm-1,Z=2,the final R = 0.0694 and wR = 0.1543 for 3034 observed reflections(I2σ(I)).In the title complex,the two Co(Ⅱ) ions are in different coordination environments with distorted octahedral and trigonal bipyramidal geometries,respectively.The Co atoms are linked together through hexadentate bptc ligands,giving rise to 2D layers which are bridged by the bix ligands into a 3-D supramolecular network.Magnetic susceptibilities of 1 reveal weak antiferromagnetic exchange interactions between the adjacent Co(Ⅱ) ions.
文摘The title compound C18H16N4O3 (Mr = 336.35) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632(1), b = 7.816(1), c = 28.082(5) A,β = 96.18(1)°, V= 1665.48(51) A^3, Z= 4, Dc = 1.341 g/cm^3, F(000) = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C(11)-C(16) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0.03 A) with the dihedral angle between them of 9.8%.
文摘The effect of UV irradiation and blending with phthalate and terephthalate plasticizers on the photo-stability of Poly (4-vinyl biphenyl) was studied at different intervals of irradiation time and in presence of air. The increase in irradiation time on the photodegradation of polymer thin films caused a change in the intensity and shape of the fluorescence band. It has been found that the stability of the polymer decreases with the increase of irradiation time, and to increases with the increase of the amount of added phthalate and terephthalate plasticizers, which is evidence of polymer photodegradation. The FT-IR spectra of irradiated pure and blended polymer with phthalate and terephthalate plasticizers showed a decrease in some absorption bands and increase in the other bands, this is also another factor for the occurrence of photo degradation of the irradiated polymer. The increase in the intensity of absorption of carbonyl and hydroxyl region, indicates a possible photogegradation of polymeric chains and the formation of alcohols, aliphatic ketones and to the increase in the number of (C=C) that resulted from hydrogen abstraction during chains-scission.
文摘Novel fluorine substituted α-amino phosphonic acids containing 1,2,4-triazin- 5-one (6a-f) have been obtained from fluoroacylation of 6-(2′-amino-5′-nitrophenyl)-3-thioxo-1,2,4-triazin-5(4H)-one (1) followed by ammonilysis to give the corresponding 3-amino-derivative 3. Condensation of compound 3 with nitro/halogenated aromatic aldehydes yielded the Schiff bases 4. The simple addition of diethyl phosphonate to compound 4 produced the α-amino phosphonates 5. Acidic hydrolysis of compound 5 produced the fluorine substituted α-amino acids derivatives 6. Structures of the new compounds have been established with the help of elemental analysis and spectral measurements. Also, the products evaluated as antioxidants, where the fluorinated α-amino phosphonic acids 6 are more active than the other synthesized systems.
基金the Opening Foundation of The Biochemical Engineering Key Discipline (No.20050105) Zhejiang,China,for financial supportthe National Center for Drug Screening,Shanghai,China,for evaluation of anti-inflammatory and analgesic activity.
文摘Eighteen 2′,4′-difluoro-3-(carbamoyl)biphenyl-4-yl benzoates were synthesized from diflunisal in three steps with total yields from 72% to 86%. All compounds were identified by IR, 1^H NMR, MS and elemental analysis. The anti-inflammatory activity and analgesic activity for 18 compounds were evaluated. The preliminary assay results showed that compounds 4a and 4p exhibited potent anti-inflammatory-analgesic activity.
文摘The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356(2), b = 7.0761(11), c = 20.539(3) A, β = 105.723(4)°, V= 1868.5(5) A3 and Z = 4.
基金This work was supported by the Phytochemistry Key Laboratory of Shaanxi Province (No. 02js40)
文摘The title compound (C16H15N3O2, Mr= 281.31) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the C=N double bond. It crystallizes in the monoclinic system, space group P2 1/c with a = 11.150(3), b = 9.906(3), c = 13.624(4) A, β = 106.360(4)°, V= 1443.9(7) ,A^3, Z = 4, Dc = 1.294 g/cm^3, F(000) = 592,μ(MoKa) = 0.088 mm ^-1, R = 0.0577 and wR = 0.1214. Of the 5766 total reflections, 2540 were unique. In the molecule there exist two different planes of pyrazoline and O(2)-C(10) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0026 A) with the dihedral angle between them of 6.3°.
基金This work is sponsored by the National Natural Science Foundation of China (No. 59473901).
文摘A new monomer of 4, 4-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA), 4, 4'-biphenyl-bis-[4-phthalazin-1(2H)-one], 4, 4- difluorodiphenylketone (DFK). The monomer and copolymer were characterized by FT-IR and 1H-NMR. DSC and TGA were used to the novel polymer.
文摘Six N-alkyl-4'-methyl-1,1'-biphenyl-2-sulfonamides were synthesized facilely and efficiently from low cost and readily available benzenesulfonyl chloride and C1-C4 fatty amines via linking DoM reaction with Suzuki reaction.The structures of the new compounds synthesized were confirmed by elemental analysis,IR,1H NMR and MS.This new method makes a feature of low cost and readily available starting material,fewer steps,mild condition,easiness to operate and higher yield.