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Hydrothermal Synthesis and Crystal Structure of One 3D Coordination Polymer of Cobalt(II) Achieved from 1,1′-Biphenyl-2,2′,6,6′-tetracarboxylic Acid Ligand 被引量:3
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作者 梅崇珍 杨光瑞 李凯慧 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2013年第2期225-230,共6页
A new three-dimensional coordination polymer {[Co(BPTC)0.5(bix)]′(H2O)}n (1, H4BPTC = 1,1′-biphenyl-2,2′,6,6′-tetracarboxylic acid, bix = 1,3-bis(imidazol-l-ylmethyl)-benzene) has been synthesized by the... A new three-dimensional coordination polymer {[Co(BPTC)0.5(bix)]′(H2O)}n (1, H4BPTC = 1,1′-biphenyl-2,2′,6,6′-tetracarboxylic acid, bix = 1,3-bis(imidazol-l-ylmethyl)-benzene) has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, and single-crystal X-ray analysis. The crystal is of orthorhombic, space group Pbcn with a = 13.2975(10), b = 13.8424(12), c = 22.6367(17) A, CoC22H19N4Os, Mr = 478.34, V = 4166.7(6) A3, Dc = 1.525 g/cm^3, F(000) = 1968,μ = 0.867 mm^-1, S = 1.023 and Z = 8. The final R = 0.0683 and wR = 0.1529 for 3655 observed reflections with I 〉 20(I). In the title complex, the 2D Co-BPTC layer is formed through self-assembly of Co(II) ions and bridging BPTC4-ligands in a molar ratio of 2:1. The metal-organic lattice layers are further united together through the second bridging ligand bix to form a 3D metal-organic framework. The thermal stability of the title complex was studied by thermal gravimetric (TG) and differential thermal analysis (DTA). 展开更多
关键词 cobalt(Ⅱ) 1 1′-biphenyl-2 2 6 6′-tetracarboxyl acid 3D coordination polymer
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联苯吡菌胺关键中间体3′,4′-二氯-5-氟-1,1′-联苯-2-胺的合成
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作者 黄晓瑛 尚宇 +2 位作者 王威 王列平 毛明珍 《世界农药》 CAS 2024年第1期38-41,49,共5页
为获得联苯吡菌胺关键中间体3′,4′-二氯-5-氟-1,1′-联苯-2-胺的适合工业化生产工艺路线,对其合成工艺进行了优化。以3,4-二氯溴苯和2-溴-4-氟苯胺为原料,经格氏和Suzuki偶联2步反应合成了3′,4′-二氯-5-氟-1,1′-联苯-2-胺,其结构经... 为获得联苯吡菌胺关键中间体3′,4′-二氯-5-氟-1,1′-联苯-2-胺的适合工业化生产工艺路线,对其合成工艺进行了优化。以3,4-二氯溴苯和2-溴-4-氟苯胺为原料,经格氏和Suzuki偶联2步反应合成了3′,4′-二氯-5-氟-1,1′-联苯-2-胺,其结构经1H NMR、MS表征确证,并对合成条件进行了优化。优化条件下,3′,4′-二氯-5-氟-1,1′-联苯2-胺合成总收率61.9%,纯度98%。该工艺成本低,收率高,具有工业化生产前景。 展开更多
关键词 3′ 4′-二氯-5-氟-1 1′-联苯-2-胺 合成 联苯吡菌胺
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Extraction Equilibria of Trimellitic and [ 1,1′-Biphenyl]-2,2′-dicarboxylic Acid with 1-Octanol, 50%TBP, and 10%TRPO in Kerosene 被引量:2
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作者 周智勇 秦炜 戴猷元 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2008年第6期867-870,共4页
To explore the feasibility of extracting aromatic acid products from oxidizing coal, two aromatic acids, trimellitic and [1,1′-biphenyl]-2,2′-dicarboxylic acid, were selected as the solutes, and the extraction equil... To explore the feasibility of extracting aromatic acid products from oxidizing coal, two aromatic acids, trimellitic and [1,1′-biphenyl]-2,2′-dicarboxylic acid, were selected as the solutes, and the extraction equilibrium of the acids were studied with 1-octanol, 50% tributyl phosphate (TBP) in kerosene, and 10% trialkylphosphine oxide (TRPO) in kerosene. The results showed that the degree of extraction of [1,1′-biphenyl]-2,2′-dicarboxylic acid was larger than that of trimellitic acid for all of the solvent, and the extraction capacity with TRPO is more effective than the one with TBP. The extraction behavior of aromatic polyacid is different from that of carboxylic acid, and the reactive extraction function of aromatic acids with TBP and TRPO is not as effective as that of carboxylic acid. 1-octanol could be used to remove [1,1′-biphenyl]-2,2′-dicarboxylic acid from the mixture of trimellitic acid and [1,1′-biphenyl]-2,2′-dicarboxylic acid. Because the weak hydrogen bond association exists between -OH in 1-octanol and -COOH in aromatic acid, the extractive selectivity of [ 1, 1′-biphenyl]-2,2′-dicarboxylic to trimellitic acid depends on the stoichiometric ratio. 展开更多
关键词 trimellitic acid [1 1′-biphenyl]-2 2′-dicarboxylic acid extraction equilibrium 1-octanol TBP and TRPO
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HPLC-MS测定奥美沙坦酯中有关基因毒性杂质 被引量:2
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作者 栾保磊 徐新军 +2 位作者 梁桂挺 游孟梦 刘国柱 《中国药科大学学报》 CAS CSCD 北大核心 2019年第3期325-329,共5页
建立一种直接测定奥美沙坦酯中基因毒性杂质5-(4′-溴甲基联苯-2-基)四氮唑和5-(4′-二溴甲基联苯-2-基)四氮唑的液相色谱-质谱联用方法。采用色谱柱AgilentZorbaxEclipsePlusC18(250mm×4.6mm,5μm),以0.1%甲酸水溶液-乙腈为流动相... 建立一种直接测定奥美沙坦酯中基因毒性杂质5-(4′-溴甲基联苯-2-基)四氮唑和5-(4′-二溴甲基联苯-2-基)四氮唑的液相色谱-质谱联用方法。采用色谱柱AgilentZorbaxEclipsePlusC18(250mm×4.6mm,5μm),以0.1%甲酸水溶液-乙腈为流动相;在电喷雾正离子模式下,对m/z315和m/z395离子进行选择性监测。5-(4′-溴甲基联苯-2-基)四氮唑和5-(4′-二溴甲基联苯-2-基)四氮唑的质量浓度分别在0.0094~0.5610μg/mL和0.0182~0.5475μg/mL范围内与峰面积呈良好线性关系;定量限分别为9.35和18.25ng/mL;检测限分别为3.12和6.08ng/mL;平均回收率分别为96.5%(n=9,RSD=4.8%)和98.0%(n=9,RSD=5.1%)。本法操作简便、专属性好、准确度高,可用于奥美沙坦酯中基因毒性杂质5-(4′-溴甲基联苯-2-基)四氮唑和5-(4′-二溴甲基联苯-2-基)四氮唑的检测。 展开更多
关键词 奥美沙坦酯 液相色谱-质谱联用 基因毒性杂质 5-(4′-溴甲基联苯-2-基)四氮唑 5-(4′-二溴甲基联苯-2-基)四氮唑
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5-(4'-甲基联苯-2-基)-1H-四唑的合成研究进展 被引量:2
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作者 吴泰志 张福利 谢美华 《精细化工中间体》 CAS 2008年第5期5-7,10,共4页
5-(4'-甲基联苯-2-基)-1H-四唑是血管紧张素Ⅱ受体拮抗剂的关键原料,综述其合成方法的研究进展。
关键词 5-(4′-甲基联苯-2-基)-1H-四唑 合成 综述
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