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二苯基膦乙酸合成方法的改进 被引量:1
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作者 郭孟萍 何仁 《化学试剂》 CAS CSCD 北大核心 2004年第2期97-98,共2页
改进了二苯基膦乙酸的合成方法。用萃取法代替减压蒸馏法分离中间物方便、可靠。
关键词 二苯基膦乙酸 合成技术 配位体 萃取法 减压蒸馏法 催化剂
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二苯基膦乙酸钯催化Suzuki偶联反应合成联苯类含氟液晶 被引量:2
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作者 夏永涛 何仁 +3 位作者 王继华 宋有永 周银波 崔明 《应用化学》 CAS CSCD 北大核心 2007年第5期489-493,共5页
以4-(反-4′-正烷基环己基)环己酮和溴苯为起始原料经格氏反应、脱水、催化氢化、构象转化、溴代,合成了4-[反-4-′(反-4″-正烷基环己基)-环己基]溴苯(5)。在二苯基膦乙酸钯催化下由化合物5与含氟苯硼酸偶联,合成了6个联苯类含氟液晶... 以4-(反-4′-正烷基环己基)环己酮和溴苯为起始原料经格氏反应、脱水、催化氢化、构象转化、溴代,合成了4-[反-4-′(反-4″-正烷基环己基)-环己基]溴苯(5)。在二苯基膦乙酸钯催化下由化合物5与含氟苯硼酸偶联,合成了6个联苯类含氟液晶化合物。以4-(反-4′-正烷基环己基)环己酮计,纯化处理后的总收率约50%。采用了DMF、叔丁醇钾体系,实现了环己烷顺、反异构体构型转换,使得反式-4-(反式-4′-正烷基环己基)-环己基苯(4)的收率达到82%,并对环己烷构型转换可能的机理进行了探讨。目标化合物经GC-MS、1H NMR测试技术表征,证明得到了预期的结果。DSC分析表明,该类液晶化合物有很高的清亮点和较宽的介晶相变温度。 展开更多
关键词 液晶化合物 SUZUKI偶联反应 二苯基膦乙酸 配位催化
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Synthesis and Crystal Structure of Dinuclear Copper Cluster Compound [Cu(dtp)PPh_3]_2
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作者 陈秋华 黄建全 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1994年第2期102-104,共3页
The title compound [Cu(dtp) PPh3]2 (dtp=S2,P(OEt)2) was prepared by heating the mononuclear compound Cu(dtp)(PPh3)2 in CH3CN solution.It crystallizes in the triclinic space group P1 with parameters a=9.71 6(5),b=11.02... The title compound [Cu(dtp) PPh3]2 (dtp=S2,P(OEt)2) was prepared by heating the mononuclear compound Cu(dtp)(PPh3)2 in CH3CN solution.It crystallizes in the triclinic space group P1 with parameters a=9.71 6(5),b=11.026(5),c=12.475(4) A.α=78.16(3)°,β=102. 64(4), γ=114.34(4)°,V=1178(1)A 3,Z=1,Dc=1.44 g/cm3,MoKα(λ=0.71069 A) μ=12. 48cm-1,F(000)=528.Final R=0.041.Rω= 0. 052 for 3653 unique intensity data(I≥3σ(I)).The molecule of the title compound can be viewed as a centrosymmetric dimer with two[Cu(dtp)(PPh3)] units,which are bridged by two S atoms belonging to the dtp ligands.The exact planar[Cu2S2] core and two[CuS2P] four-membered rings form a chair conformation.The Cu…Cu distance is 2.991(5) A. 展开更多
关键词 SYNTHESIS crystal structure copper cluster dinuclear compound
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Synthesis and Crystal Structure of a Dicopper(Ⅰ) Complex with Bis(diphenylphosphino)methane and Diethyldithiocarbamate
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作者 HUANG Shao-Bin② SITU Yue (Department of Applied Chemistry, South China University of Technology, Guangzhou, Guangdong 510640, China) 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 北大核心 2003年第3期260-264,共5页
The title complex [Cu2(-dppm)2(-Et2dtc)](ClO4)EtOH0.25H2O (dppm = bis- (diphenylphosphino)methane, Et2dtc = diethyldithiocarbamate) has been synthesized and characterized by single-crystal X-ray diffraction analysis. ... The title complex [Cu2(-dppm)2(-Et2dtc)](ClO4)EtOH0.25H2O (dppm = bis- (diphenylphosphino)methane, Et2dtc = diethyldithiocarbamate) has been synthesized and characterized by single-crystal X-ray diffraction analysis. The crystal structure is of monoclinic, space group C2/c with a = 42.587(1), b = 14.1653(4), c = 20.5649(5) ? = 105.945(1)? V =11928.6 3, C57H60.5ClCu2NO5.25P4S2, Mr = 1194.09, Z = 8, Dc = 1.330 g/cm3, (MoK) = 0.98 mm-1 and F(000) = 4948. A total of 15243 reflections were collected, of which 7322 were unique. The structure was refined to R = 0.0739 and wR = 0.1846 for 5135 observed reflections with I > 2(I). The crystal structure consists of the complex cation [Cu2(-dppm)2(-Et2dtc)]+, anion ClO4- and solvate H2O and EtOH, where the dinuclear Cu(Ⅰ) atoms are bridged doubly by two dppm ligands and singly by Et2dtc to give three five-membered rings. The Cu(Ⅰ) atom is in an approxi- mately trigonal-planar environment with the P2S chromophore. The short Cu贩稢u separation (2.7111 ? suggests the presence of metal-metal contact. 展开更多
关键词 synthesis crystal structure dicopper complex DIETHYLDITHIOCARBAMATE
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Synthesis and Structure of Di[bis(diphenylphosphino)ethane] Copper(Ⅱ) Dinitrate
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作者 LIN Kun-Hua YANG Rui-Na +2 位作者 CAI Dong-Mei JIN Dou-Man(Henan Institute of Chemistry, Zhengzhou 450003)(Zhengzhou Grain College, Zhengzhou 450052)CHENG Liao-Rong LUO Bao-Sheng(Analysis and Testing Centre, Wuhan University, Wuhan 430072) 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1996年第5期337-340,共4页
The complex[Cu (dppe)2](NO3)2 was prepared by the reaction of copper(Ⅱ) nitrate with bis(diphenylphosphino) ethane(dppe) in methanol and its crystal structure was determined by X-ray diffraction.The structure was so... The complex[Cu (dppe)2](NO3)2 was prepared by the reaction of copper(Ⅱ) nitrate with bis(diphenylphosphino) ethane(dppe) in methanol and its crystal structure was determined by X-ray diffraction.The structure was solved by direct methods and refined by block-diagonal and full-matrix least-squares methods to a final R of 0.043 for 4085 independent reflections of I>3σ(I).The crystal is monoclinic, space group P21/n,Mr=984.41 with cell parameters a=12.896(2),b=22.250(4),c=17.512(5)A,β=101.6(3)°, V=4922.3 A3,Z=4,Dc=1.590 g/cm3,F(000)=1900,μ=10.573 cm-1. In this complex, C52H48CuN2O6P4, dppe functions as a bidentate chelate ligand. The four phosphorus atoms from two dppe are coordinated to the distorted tetrahedral copper. 展开更多
关键词 copper complex crystal structure SYNTHESIS
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羧基膦-钯-酸体系催化烯烃氢酯基化反应 被引量:3
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作者 周宏英 吴彪 +2 位作者 吕士杰 陈静 傅宏祥 《分子催化》 EI CAS CSCD 1996年第1期13-18,共6页
以钯-膦-酸体系催化烯烃氢酯基化的反应日显重要,而膦配体是决定此反应的重要因素,用二苯基膦乙酸(DPA)为配体的钯催化剂体系,对烯烃的氢酯基化反应作了研究。对影响反应的各种因素如反应温度、反应压力、不同的溶剂、膦配体... 以钯-膦-酸体系催化烯烃氢酯基化的反应日显重要,而膦配体是决定此反应的重要因素,用二苯基膦乙酸(DPA)为配体的钯催化剂体系,对烯烃的氢酯基化反应作了研究。对影响反应的各种因素如反应温度、反应压力、不同的溶剂、膦配体及酸助剂的量等作了考察,发现此配体对烯烃的区域选择性有改善。并用此催化体系对不同结构的烯烃进行了研究,发现有如下的活性顺序:环烯烃>直链端烯>直链内烯。 展开更多
关键词 氢酯基化 烯烃 二苯基膦乙酸 催化剂 羧酸酯
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