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双格氏试剂法合成4,4’-二(二苯基膦基)联苯
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作者 姚骏 齐磊 +3 位作者 毕峰 洪啸 柳利 李法宝 《湖北大学学报(自然科学版)》 CAS 2015年第4期387-390,共4页
以4-溴联苯为原料,通过卤代反应获得二溴联苯后,与活泼金属镁反应制备双格氏试剂,再与二苯基氯化磷反应一步合成目标化合物4,4’-二(二苯基膦基)联苯.采用核磁共振谱(1H、13C、31P NMR)、傅里叶变换红外光谱(FT-IR)、液质联用飞行时间质... 以4-溴联苯为原料,通过卤代反应获得二溴联苯后,与活泼金属镁反应制备双格氏试剂,再与二苯基氯化磷反应一步合成目标化合物4,4’-二(二苯基膦基)联苯.采用核磁共振谱(1H、13C、31P NMR)、傅里叶变换红外光谱(FT-IR)、液质联用飞行时间质谱(LC-MS TOF)等对目标化合物进行表征,表征结果与结构相吻合.与传统的合成法相比,该法具有操作简便、反应条件温和、原料成本低等优点. 展开更多
关键词 4 4’-二(二苯基膦基)联苯 双格氏试剂 合成 表征
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Synthesis, Crystal Structure, and Topology Analysis of One Novel Interpenetrated 2D Cobalt Coordination Polymer, {[Co(HTCB)(4,4'-btb)]·H_2O}_n 被引量:3
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作者 高艳 范黎明 +2 位作者 宋维阔 刘新征 张修堂 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2014年第9期1333-1338,共6页
One novel cobalt coordination polymer, {[Co(HTCB)(4,4'btb)]'HzO}n (1, H3TCB = 1,3,5-tris(4-carboxyphenyl)benzene, 4,4'-btb = 4,4'-bis(1,2,4-triazol-3-yl)biphenyl), has been synthesized and characterized ... One novel cobalt coordination polymer, {[Co(HTCB)(4,4'btb)]'HzO}n (1, H3TCB = 1,3,5-tris(4-carboxyphenyl)benzene, 4,4'-btb = 4,4'-bis(1,2,4-triazol-3-yl)biphenyl), has been synthesized and characterized by elemental analysis, IR, powder X-ray diffraction (PXRD), and thermogravimetric (TG) analyses. X-ray diffraction analysis reveals that complex 1 is a 2D 2-fold interpenetrated {44,62}-sql [Co(HTCB)(4,4'-btb)] sheet based on the 1D [Co(HTCB)]n chains and 1D [Co(4,4'-btb)]n chains. The crystal of 1 crystallizes in triclinic, space group P1 with a = 9.529(12), b = 13.914(16), c = 14.906(17) A, V= 1903(4) A3, Z = 2, C45H34N6CoO71 Mr= 829.71, Dc = 1.448 g/cm3, F(000) = 858 andμ(MoKa) = 0.514 mm-1. The final R = 0.0655 and wR = 0.1136 for 6603 observed reflections with 1 〉 2a(/) and R = 0.1136 and wR = 0.1747 for all data. 展开更多
关键词 1 3 5-tris(4-carboxyphenyl)benzene 4 4'-bis(1 2 4-triazol-3-yl)biphenyl cobalt interpenetrated topology
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Crystal Structure of an Octanuclear Sandwich Cluster of Silver(I) and 4,4'-Bis(2,5-dimethylstyryl)biphenyl 被引量:1
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作者 刘淑芹 宁桂玲 +2 位作者 张雄福 小中·尚 宗像·惠 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2006年第9期1259-1262,共4页
Reaction of the oligo(phenylenevinylene) 4,4'-bis(2,5-dimethylstyryl)biphenyl (bdb) with CF3CO2Ag in benzene gave a novel octanuclear sandwich cluster [Ags(bdb)2(C6H6)2(CF3CO2)8]·2C6H6 (1). The clu... Reaction of the oligo(phenylenevinylene) 4,4'-bis(2,5-dimethylstyryl)biphenyl (bdb) with CF3CO2Ag in benzene gave a novel octanuclear sandwich cluster [Ags(bdb)2(C6H6)2(CF3CO2)8]·2C6H6 (1). The clusters are packed on each other through strong n-n interactions to form ^1D 'brick' chains, between which the solvated benzene molecules are located. TG analysis showed that cluster 1 could completely liberate the guest benzene molecules at 105℃ and the coordinated benzene molecules at 180 ℃. In solid state, cluster 1 exhibits fluorescence, and the emission band is red-shifted compared with that of free ligand bdb. 展开更多
关键词 silver(Ⅰ) complex octanuclear cluster 4 4'-bis(2 5-dimethylstyryl)biphenyl oligo(phenylenevinylene)
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Enantioseparation of Racemic Anti-hepatitis New Drug Bicyclol with Crystallization 被引量:2
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作者 Wei HU Yan LI Chun Zhen ZHANG 《Chinese Chemical Letters》 SCIE CAS CSCD 2005年第11期1471-1473,共3页
The enantioseparation of anti-hepatitis new drug (±)-bicyclol was performed by optically active alkaloid. The alcoholic acid, the hydrolysate of bicyclol was reacted with optically active alkaloid, such as bruc... The enantioseparation of anti-hepatitis new drug (±)-bicyclol was performed by optically active alkaloid. The alcoholic acid, the hydrolysate of bicyclol was reacted with optically active alkaloid, such as brucine, strychnine, quinidine etc., the diastereoisomeric salts were obtained by fractional recrystallization, then separately decomposed and esterified to obtain the two enantiomers of bicyclol. The pharmacological study showed that the effect of (-)-bicyclol was more potent than racemic bicyclol two times and the potency of (+)-bicyclol was incative. 展开更多
关键词 (±)-bicyclol 4 4'-dimethoxy-2 3 2 3'-bis(methylenedioxy)-6-hydroxymethyl-6'-methoxy-carbonyl biphenyl anti-hepatitis resolution.
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