A new Na(I) coordination polymer,[Na2(Hpimdc)(H2 pimdc)(phen)2]n(1), has been synthesized by the reaction of NaOH with 2-propyl-4,5-imidazoledicarboxylic acid(H3 pimdc)and 1,10-phenanthroline(phen). The Na(I) coordina...A new Na(I) coordination polymer,[Na2(Hpimdc)(H2 pimdc)(phen)2]n(1), has been synthesized by the reaction of NaOH with 2-propyl-4,5-imidazoledicarboxylic acid(H3 pimdc)and 1,10-phenanthroline(phen). The Na(I) coordination polymer 1 was characterized by single-crystal X-ray diffraction analysis and elemental analysis. In 1, the bridged ligand H3 pimdc adopts two modes(singly deprotonated and doubly deprotonated) to coordinate with the Na(I) ion.The Na(1) ion is six-coordinated with three N atoms from a phen ligand and a H2 pimdc ligand,three O atoms from a Hpimdc ligand and two other different H2 pimdc ligands. The Na(2) ion is also six-coordinated with three N atoms from a phen ligand and a Hpimdc ligand, three O atoms from a H2 pimdc ligand and other two different Hpimdc ligands. Complex 1 exhibits a 1 D chain structure built up by μ-H2 pimdc-and μ-Hpimdc2-ligands. The antitumor activities of complex 1 against human SGC7901, A549 and H08910 cells have been tested.展开更多
A novel series of para-diiodobenzene derivatives, 3,6-diiodo-4,5-dialkyl-phthalic acid dimethyl esters, were prepared via cycloaddition of two TMS-substituted alkynes and dimethyl acetylenedicarboxylate, which was med...A novel series of para-diiodobenzene derivatives, 3,6-diiodo-4,5-dialkyl-phthalic acid dimethyl esters, were prepared via cycloaddition of two TMS-substituted alkynes and dimethyl acetylenedicarboxylate, which was mediated by zirconocene. After iodination, three new compounds of 3,6-diiodo-4,5-dimethyl(dipropyl, dibutyl)-phthalic acid dimethyl esters (3a, 3b, 3c) were synthesized in high region-selectivity and yields, and characterized by NMR. The crystal structures were determined by single-crystal X-ray diffraction. The crystal of 3a (C12H121204, Mr = 474.02) belongs to the triclinic system, space group Pi with a = 7.6238(10), b = 9.4571(12), c = 10.8221(14) A, a = 66.611(10), fl = 88.511(12), 7 : 77.604(11)% V= 697.93(16) A3, Z= 2, F(000) = 444, Dc = 2.256 mg/m3, g = 4.509 mm-1, T=133(2) K, S = 1.014, R = 0.0229 and wR = 0.0547 for 2644 observed reflections with I 〉 20(/); the crystal of 3b (C16H201204, Mr - 530.12) is of triclinic system, space group Pi with a = 9.4122(19), b = 10.626(2), c = 11.353(2) A, a = 97.90(3), fl = 113.83(3), y = 110.22(3)°, V= 922.6(3) A3, Z- 2, F(000) = 508, Dc - 1.908 mg/m3, g = 3.422 mm-1, T = 113(2) K, S = 1.115, R = 0.0428 and wR = 0.1072 for 3971 observed reflections with I〉 20(/); the crystal of 3c (ClsH241204, Mr = 558.17) belongs to the monoclinic system, space group P21/c with a = 26.396(2), b = 8.7560(8), c = 25.7970(18) A, fl = 91.721(4)o, V= 5959.6(8) A3, Z = 12, F(000) = 3240, Dc = 1.866 mg/m3,/z = 3.184 mm-l, T= 113(2) K, S = 1.154, R = 0.0424 and wR = 0.0766 for 13056 observed reflections with I 〉 20(/).展开更多
Enantiomerically pure syn-4,5-dihydroxy carboxylic acid lactones were prepared by microbial reduction of acyl lactones with resting cell of Aspergillus niger.
以3,4-二甲基苯胺为原料,经与水合氯醛、盐酸羟胺缩合,浓H2SO4作用下环合,碱性双氧水条件下进一步氧化开环合成2-氨基-4,5-二甲基苯甲酸,三步反应的总收率为34.3%.产物结构经傅里叶变换红外光谱(FT-IR)、核磁共振氢谱(1 H NMR)表征,证...以3,4-二甲基苯胺为原料,经与水合氯醛、盐酸羟胺缩合,浓H2SO4作用下环合,碱性双氧水条件下进一步氧化开环合成2-氨基-4,5-二甲基苯甲酸,三步反应的总收率为34.3%.产物结构经傅里叶变换红外光谱(FT-IR)、核磁共振氢谱(1 H NMR)表征,证明了结构的正确性.展开更多
A new one-dimensional Ni(Ⅱ) coordination polymer [Ni(L)(cis-1,4- chdc)]n·1.25nH2O has been synthesized under hydrothermal conditions by using 1,4-cyclohexanedicarboxylic acid (1,4-H2chdc) and 2-(3-fluor...A new one-dimensional Ni(Ⅱ) coordination polymer [Ni(L)(cis-1,4- chdc)]n·1.25nH2O has been synthesized under hydrothermal conditions by using 1,4-cyclohexanedicarboxylic acid (1,4-H2chdc) and 2-(3-fluorophenyl)- 1H-imidazo [4,5-f] [ 1,10]phenanthroline (L). Crystallographic data for the compound: triclinic, space group Pi with a = 8.777(2), b = 10.662(2), c = 13.799(3) A, a = 89.480(4), β = 73,933(3), γ = 81.980(4)°, V = 1228.2(5) A3, Z = 2, C27H22.50FN4NiO5.25, Mr = 568.70, Dc = 1.527 g/cm3, F(000) = 583,μ(MoKα) = 0.846 mm-1, R = 0.0634 and wR = 0.1465. Neighboring Ni(Ⅱ) atoms are linked by the cis-1,4-chdc ligands to generate a one-dimensional chain structure. The π-π interactions between the L ligands of neighboring chains led to the formation of a two-dimensional supramolecular layer. The elemental analysis, IR spectrum and TG of the compound have been studied.展开更多
基金supported by the National Natural Science Foundation of China(No.21171132)the Project of Shandong Province Higher Educational Science and Technology Program(J14LC01)Science Foundation of Weifang
文摘A new Na(I) coordination polymer,[Na2(Hpimdc)(H2 pimdc)(phen)2]n(1), has been synthesized by the reaction of NaOH with 2-propyl-4,5-imidazoledicarboxylic acid(H3 pimdc)and 1,10-phenanthroline(phen). The Na(I) coordination polymer 1 was characterized by single-crystal X-ray diffraction analysis and elemental analysis. In 1, the bridged ligand H3 pimdc adopts two modes(singly deprotonated and doubly deprotonated) to coordinate with the Na(I) ion.The Na(1) ion is six-coordinated with three N atoms from a phen ligand and a H2 pimdc ligand,three O atoms from a Hpimdc ligand and two other different H2 pimdc ligands. The Na(2) ion is also six-coordinated with three N atoms from a phen ligand and a Hpimdc ligand, three O atoms from a H2 pimdc ligand and other two different Hpimdc ligands. Complex 1 exhibits a 1 D chain structure built up by μ-H2 pimdc-and μ-Hpimdc2-ligands. The antitumor activities of complex 1 against human SGC7901, A549 and H08910 cells have been tested.
文摘A novel series of para-diiodobenzene derivatives, 3,6-diiodo-4,5-dialkyl-phthalic acid dimethyl esters, were prepared via cycloaddition of two TMS-substituted alkynes and dimethyl acetylenedicarboxylate, which was mediated by zirconocene. After iodination, three new compounds of 3,6-diiodo-4,5-dimethyl(dipropyl, dibutyl)-phthalic acid dimethyl esters (3a, 3b, 3c) were synthesized in high region-selectivity and yields, and characterized by NMR. The crystal structures were determined by single-crystal X-ray diffraction. The crystal of 3a (C12H121204, Mr = 474.02) belongs to the triclinic system, space group Pi with a = 7.6238(10), b = 9.4571(12), c = 10.8221(14) A, a = 66.611(10), fl = 88.511(12), 7 : 77.604(11)% V= 697.93(16) A3, Z= 2, F(000) = 444, Dc = 2.256 mg/m3, g = 4.509 mm-1, T=133(2) K, S = 1.014, R = 0.0229 and wR = 0.0547 for 2644 observed reflections with I 〉 20(/); the crystal of 3b (C16H201204, Mr - 530.12) is of triclinic system, space group Pi with a = 9.4122(19), b = 10.626(2), c = 11.353(2) A, a = 97.90(3), fl = 113.83(3), y = 110.22(3)°, V= 922.6(3) A3, Z- 2, F(000) = 508, Dc - 1.908 mg/m3, g = 3.422 mm-1, T = 113(2) K, S = 1.115, R = 0.0428 and wR = 0.1072 for 3971 observed reflections with I〉 20(/); the crystal of 3c (ClsH241204, Mr = 558.17) belongs to the monoclinic system, space group P21/c with a = 26.396(2), b = 8.7560(8), c = 25.7970(18) A, fl = 91.721(4)o, V= 5959.6(8) A3, Z = 12, F(000) = 3240, Dc = 1.866 mg/m3,/z = 3.184 mm-l, T= 113(2) K, S = 1.154, R = 0.0424 and wR = 0.0766 for 13056 observed reflections with I 〉 20(/).
文摘Enantiomerically pure syn-4,5-dihydroxy carboxylic acid lactones were prepared by microbial reduction of acyl lactones with resting cell of Aspergillus niger.
基金Supported by the Institute Foundation of Siping City (No. 2009011)
文摘A new one-dimensional Ni(Ⅱ) coordination polymer [Ni(L)(cis-1,4- chdc)]n·1.25nH2O has been synthesized under hydrothermal conditions by using 1,4-cyclohexanedicarboxylic acid (1,4-H2chdc) and 2-(3-fluorophenyl)- 1H-imidazo [4,5-f] [ 1,10]phenanthroline (L). Crystallographic data for the compound: triclinic, space group Pi with a = 8.777(2), b = 10.662(2), c = 13.799(3) A, a = 89.480(4), β = 73,933(3), γ = 81.980(4)°, V = 1228.2(5) A3, Z = 2, C27H22.50FN4NiO5.25, Mr = 568.70, Dc = 1.527 g/cm3, F(000) = 583,μ(MoKα) = 0.846 mm-1, R = 0.0634 and wR = 0.1465. Neighboring Ni(Ⅱ) atoms are linked by the cis-1,4-chdc ligands to generate a one-dimensional chain structure. The π-π interactions between the L ligands of neighboring chains led to the formation of a two-dimensional supramolecular layer. The elemental analysis, IR spectrum and TG of the compound have been studied.