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MCM-41固载胺钯配合物的制备及对Heck反应催化性能的研究 总被引:1,自引:0,他引:1
以MCM-41分子筛作为固载材料, 经氨基功能化后与各种钯化合物形成一系列MCM-41载钯配合物, 采用XRD, XPS等技术对其结构及表面性能进行了表征, 研究了催化剂的制备条件等因素对催化Heck芳基化反应性能的影响; 以共轭烯烃和各种芳基碘的Heck芳基化反应考察了MCM~NH2•Pd(0, II)配合物的催化性能. 结果表明, MCM-41的结构没有被破坏, MCM~NH2载钯配合物具有较高的催化活性和立体选择性, 在较低的温度(70~90 ℃)下, 可高产率地生成一系列取代的反式产物. 相似文献
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MCM-41分子筛固载腈钯配合物的合成及其催化Heck偶联反应的性能 总被引:1,自引:0,他引:1
合成了MCM-41分子筛固载腈钯(0,Ⅱ)配合物催化剂,并利用XPS、FT-Raman等技术对催化剂进行了表征.研究表明,MCM-41分子筛载体上的-CN基可通过叁键上的π电子对与Pd发生弱配位.MCM-(CH2)3CN·Pd(O)具有良好的催化性能和稳定性,在反应温度70℃、DMF-Et3N的存在下,对催化各种碘代芳烃与共轭烯烃的Heck偶联反应均较有效,高产率且高立体选择地生成了一系列取代的反式产物,产物分离收率达到84%以上. 相似文献
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偕胺肟纤维-钯(Ⅱ)配合物的制备及其对Heck反应的催化性能研究 总被引:1,自引:0,他引:1
以聚丙烯腈纤维为基体,制备了偕胺肟纤维-钯(Ⅱ)配合物,采用FTIR、XPS等物理化学手段对其结构进行了表征.本文研究考察了该配合物在不同反应条件下对碘苯与苯乙烯的Heck反应的催化性能,结果显示:偕胺肟纤维-钯(Ⅱ)配合物在较温和的条件下即可很好的催化Heck反应,经重复使用8次后,1,2-二苯乙烯的产率仍达80%以上,并且反应结束后催化剂易于从反应体系中分离.对于其它不同底物之间的Heck反应,偕胺肟纤维-钯(Ⅱ)配合物同样显示较好的催化性能. 相似文献
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摘要:本文利用2-吡啶甲醛和乙二胺制得乙二胺-2-吡啶甲醛席夫碱配体,再与钯盐作用制得乙二胺-2-吡啶甲醛席夫碱钯配合物。运用红外光谱、核磁共振、质谱、元素分析、ICP等分析手段对乙二胺-2-吡啶甲醛席夫碱配体及其钯配合物进行了表征,提出了乙二胺-2-吡啶甲醛席夫碱钯配合物的结构,并对其在Heck反应中的催化性能进行了研究。 相似文献
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壳聚糖钯催化Heck反应合成肉桂酸丁酯的研究 总被引:12,自引:0,他引:12
以天然高分子壳聚糖为载体,制得了用于Heck反应的壳聚糖钯配合物多相催化剂,用XPS对其结构进行了表征,并利用正交实验方法考察了原料配比、缚酸剂三乙胺的用量、反应温度、反应时间和催化剂的用量对碘代苯与丙烯酸丁酯Heck反应的影响.结果表明:反应因素的影响大小为:反应温度>原料配比>三乙胺用量>催化剂的用量>反应时间;在最佳的反应条件下:碘代苯与丙烯酸丁酯的摩尔比为1∶1、三乙胺9mmol、催化剂0.1g(钯含量1.88×10-2mmol)时,氮气保护下140℃反应8h,肉桂酸丁酯的产率可高达99.8%.并且该催化剂对其它丙烯酸酯的Heck反应也具有良好的催化活性. 相似文献
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Jianmin Zhou Yulin Yang Lan Zhao Xiaokun Li Renxian Zhou Xiaoming Zheng 《Frontiers of Chemistry in China》2009,4(2):142-148
Using MCM-41 as the supporter, a series of MCM-41 supported amino-palladium complexes has been prepared and characterized
by XRD (X-ray diffraction) and XPS (X-ray photoelectron spectroscopy), etc. The XRD and XPS results indicate that the Pd coordinates
with the -NH2 groups on the MCM-41 surface, and the structure of MCM-41 has been not damaged. Its catalytic performance for Heck arylation
of alkene with aryl iodide shows that the catalysts have high activity and stereoselectivity in 70–90°C. The product of Heck
reaction is in E form. And the effect of the preparation condition of catalyst on the catalytic performance was examined.
Translated form Chinese Journal of Organic Chemistry, 2008, 28(5) (in Chinese) 相似文献
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Two kinds of chitosan derivatives, crosslinked chitosan and crosslinked chitosan condense with salilylaldehyde, supported palladium complexes (CL‐CTS‐Pd and CL‐S‐CTS‐Pd) were synthesized and characterized by X‐ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), differential thermal analysis (DTA), etc. These complexes are efficient catalysts for the Heck reaction under atmospheric conditions and can be easily recovered and reused. The detailed studies show that the catalyst CL‐S‐CTS‐Pd is much more efficient than CL‐CTS‐Pd under the same conditions. CL‐S‐CTS‐Pd keeps its catalytic activity in the Heck reaction of acrylic acid with iodobenzene even at a low temperature (60°C) or with tiny amounts of the catalyst (0.05 mol%Pd). Yields of making cinnamic acid were even as high as 75.3% in the Heck reaction of acrylic acid with iodobenzene using CL‐S‐CTS‐Pd that was recovered 10 times. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
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Dimitrios P. CatsoulacosBarry R. Steele Georgios A. HeropoulosMaria Micha-Screttas Constantinos G. Screttas 《Tetrahedron letters》2003,44(24):4575-4578
DAB-dendr-(NH2)32 has been modified to produce two novel dendrimeric P,N-ligands, DAB-dendr-[1,2-(NCHC6H4PPh2)]32 and DAB-dendr-[1,2-(NHCH2C6H4PPh2)]32. These were both found to activate electron rich aryl bromides in the Heck reaction. The reactions seem to proceed better in a novel solvent system consisting of an equimolar mixture of a tertiary amine with acetic acid. A marked dependence of the conversion on the [equivalents of dendrimeric ligand]/[Pd] ratio has been observed with conversion decreasing as the ratio of dendrimer equivalents to Pd increases. This phenomenon is attributed to interactions of the arms bearing the metal with neighboring ones within the dendrimer. 相似文献
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Shao-Fen Zhao Ren-Xian Zhou Yuan-Fa Yang Xiao-Ming Zheng 《Reaction Kinetics and Catalysis Letters》2003,79(2):333-340
Silica-supported palladium (0) complexes have been prepared from γ-chloropropyl triethoxysilica and γ-aminopropyl triethoxysilica
via immobilization on fumed silica, followed by reacting with ethylenediamine and salicylaldehyde, and then the reaction with
palladium chloride in ethanol and reduction with KBH4 in ethanol. They are efficient catalysts for Heck reaction of aryl iodides with alkene at 90oC. These polymeric palladium (0) catalysts can be recovered and reused without loss in activity.
This revised version was published online in June 2006 with corrections to the Cover Date. 相似文献
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Xia Xu Pu Liu San-hua Li Peng Zhang Xiang-yu Wang 《Reaction Kinetics and Catalysis Letters》2006,88(2):217-223
Summary A chitosan-supported imine palladacycle complex has been synthesized by salicyladehyde via grafting on chitosan to form chitosan-Schiff
base, followed by reacting with Li2PdCl4 in methanol. The catalyst has high activity and stereoselectivity for arylation of conjugate alkenes with aryl halides. This
chitosan-supported imine palladium catalyst can be recovered and reused. 相似文献
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综述了不对称Heck反应在天然产物合成中的应用,按照分子内和分子间的不对称Heck反应分两个方面加以介绍和总结。参考文献26篇。 相似文献
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Armandodoriano BiancoClaudia Cavarischia Angela FarinaMarcella Guiso Carolina Marra 《Tetrahedron letters》2003,44(51):9107-9109
Several naturally occurring flavonoids have been synthesised following a new proposed method based on the use of the Heck reaction. The key step involves the coupling of an aryl vinyl ketone with an aryl iodide. This procedure affords the flavonoid moiety in a single step. 相似文献
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Orhan Altan Osman Serindağ Koray Sayın Duran Karakaş 《Phosphorus, sulfur, and silicon and the related elements》2016,191(7):993-999
Novel phosphine oxides, (((3-methylpyridin-2-yl)amino)methyl)diphenylphosphine oxide (1) and diphenyl((pyrazin-2-ylamino)methyl)phosphine oxide (2), were synthesized and characterized. Phosphines ligands (3 and 4) were obtained by the reduction of 1 and 2 with AlH3, monitored by 31P NMR spectroscopy. Pd(II) complexes of 3 and 4 were synthesized and characterized (5 and 6). The catalytic activity of 5 and 6 was tested on the reaction of styrene with both activated and deactivated aryl bromides in air. The results of the catalytic experiments were discussed through DFT calculations. 相似文献
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Chieh-Keng Li 《Journal of organometallic chemistry》2011,696(23):3637-3642
The reaction of allylpalladium chloride dimer and 4,4′-bis(RfCH2OCH2)-2,2′-bpy, 1a-c, in the presence of AgOTf resulted in the synthesis of cationic complex, [Pd(η3-allyl)(4,4′-bis-(RfCH2OCH2)-2,2′-bpy)](OTf), 2a-c where Rf = C9F19 (a), C10F21 (b), C11F23 (c), respectively. The solubility curves of 2a-c which began from virtually zero below −40 °C and increased dramatically at slightly higher temperature were quantitatively measured. Upon changing from −40-90 °C there was several orders of magnitude increase of solubility for 2a-c. The cationic Pd-catalyzed Heck arylation of methyl acrylate was selected to demonstrate the feasibility of recycling usage with 2b,c as the catalyst using DMF as the solvent at 140 °C for 3 h in each run. At the end of each cycle, the product mixtures were cooled to −30 °C, and then catalysts were recovered by decantation. The products were quantified by GC analysis or by the isolated yield. The Heck reaction of C6H5I with methyl acrylate could be catalyzed by 2b with good recycling results for a total of 15 times and also with a 100% selectivity favoring the trans product. To our knowledge, this is the first example of cationic Pd-catalyzed Heck reaction under the thermomorphic mode. 相似文献