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2,2'-联吡啶桥连的双-4,4'-联吡啶哑铃型化合物的合成 总被引:5,自引:0,他引:5
二甘醇2与对甲苯磺酰氯在CH_2Cl_2中,0 ℃~r.t.及Et_3N存在下反应得2- (羟乙氧基)乙醇对甲苯磺酸酯(3),收率88%。化合物3与对叔丁基苯甲酰氯在 CH_2Cl_2中0~5 ℃及吡啶存在下反应得2-(对叔丁基苯甲酰氧基乙氧基)乙醇对 甲苯磺酸酯(4),收率96%。4与对羟苯甲醇在乙腈中及CsF/K_2CO_3存在下70 ℃ 反应得2-(对叔丁基苯甲酰氧基乙氧基)乙氧苄醇(5),收率98%。5与NBS及 PPh_3在THF中,室温下反应得化合物2-(对 丁基苯甲酰氧基乙氧基)乙氧苄溴 (6),收率95%。6与4,4'-联吡啶在乙腈中,60 ℃反应1h得N-[2-(对叔丁基 苯甲酰氧基乙氧基)乙氧苄基]-4,4'-联吡啶六氟磷酸盐(7),收率85%。7与 α,α-二(溴甲基)-2,2'-联吡啶在乙腈中,油浴60 ℃反应36h,得到标题化 合物,产率为45%。 相似文献
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以甲基咪唑(或咪唑)和N-取代芳基-3-氯丙酰胺为原料,与KPF-6经离子交换制得6个新型酰胺基功能化离子液体(2a~2c和3a~3c)。以2-溴-6-甲氧基萘与烯丙醇反应为模板反应,2或3为反应介质,考察反应的转化率和区域选择性。结果表明: 3为反应介质时,转化率和区域选择性均高于2。以溴代芳烃和烯丙醇为原料,3c为反应介质,醋酸钯催化Heck反应制得2-取代芳烃烯丙醇化合物,收率85%~89%,立体选择性均大于99%。所得产物的结构均经1H NMR, 13C NMR, IR, EI-MS和元素分析表征。 相似文献
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以DMF作溶剂,在四丁基氟化铵 (TBAF)存在下,对甲基苯基三甲硅基醚(1)和4,4'-二氯二苯砜(2)于100 ℃反应1 h,合成了4,4'-二(4-甲基苯氧基)二苯砜(3),产率为92%;加入催化量的N-溴代丁二酰亚胺(NBS)并在光照条件下,与氧气反应得到中间体-4,4'-二(4-羧基苯氧基)二苯砜(4),其产率达90%;将化合物4与二氯亚砜反应合成目标产物4,4'-二(4-氯甲酰基苯氧基)二苯砜(5),总收率为74.5%(以对甲基苯基三甲硅基醚为基准计算). 相似文献
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Fe(acac)3-Al(i-Bu)3-α,α'-联吡啶催化丙烯腈与苯乙烯共聚合 总被引:1,自引:0,他引:1
研究了Fe(acac)3-Al(i-Bu)3-α,α'-联吡啶(acac=乙酰丙酮)催化体系催化丙烯腈(AN)与苯乙烯共聚合,用元素分析和核磁共振研究了共聚物的结构,在单体比为1:1时共聚物中丙烯腈/苯乙烯含量分别为49.3%和50.7%.用凝胶渗透色谱研究了聚合物分子量和分子量分布,共聚物分子量分布较窄.动力学研究表明共聚合反应对单体浓度呈一级关系,表观活化能为57.8kJ/mol. 相似文献
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1 INTRODUCTION Self-assembly of coordination polymers fromthe basic building blocks is of considerable interestdue to their intriguing diverse architectures and po-tential applications in catalysis and advanced mater-ials, such as magnetic, optical a… 相似文献
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在DMF溶剂中合成了犤Co(H2O)4(2,2'-bipy)犦(bdc)和犤Cu(2,2'-bipy)(bdc)(H2O)犦(2H2O)(DMF)二个配合物并进行了结构解析。配合物犤Co(H2O)4(2,2'-bipy)犦(bdc)中,bdc2-以离子形式未与金属配位,但与配位水分子形成了8个氢键,从而使分子结构扩展为二维双层氢键网络。在配合物犤Cu(2,2'-bipy)(bdc)(H2O)犦(2H2O)(DMF)中,bdc2-以双单齿形式与金属离子配位,从而使分子结构扩展为一维拉链型;未配位的水分子将一维拉链扩展为二维氢键网络。 相似文献
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Chiral 2,2'-bipyridines have been reported to be highly efficient catalysts and useful building blocks of supramolecular.[1,2] Chirality of bipyridines was introduced by chiral substituents. Because 1,1'-binaphthyl (BINOL) and its derivatives belong to the most important components of asymmetric catalysts, we would like to synthesize 5,5'-and 6,6'-positions substituted chiral bipyridine-type ligands, the chiral moieties of ligands originate from enationpure 1, 1'-binapthyl units. 相似文献
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Xing Guo CHEN Chu Luo YANG Jin Gui QIN* Kyuya YAKUSHI Yasuhiro NAKAZAWA Kenji ICHIMURA Department of Chemistry Wuhan University Wuhan Institute for Molecular Science Okazaki Japan Department of Chemistry Faculty of Science Kumamoto University Kumamoto Japan 《中国化学快报》2003,(11)
Interest in nanocomposite materials is increased due to their great significance in both fundamental and applied research fields in the past two decades 1. Intercalation of organic species into lamellar inorganic solids provides a useful approach to design and synthesize inorganic-organic nanocomposite materials with novel functional properties compared with the parent compounds 2. The transition metal phosphorous trisulfides, MPS3 (M stands for a metal in +2 oxidation state), are lamellar c… 相似文献
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The two title complexes,[Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5-(NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal=3,5-dinitrosalicylate,2,2′-bipy=2,2′-bipyridine),were synthesized by the hydrothermal reaction and structurally characterized. Complex 1 crystallizes in triclinic,space group P1,a=5.581(4),b=12.071(8),c=12.88(1),α=92.10(3),β=96.73(3),γ =102.02(2)°,C17H10N4O7Cd,Mr=494.69,V=841(1)3,Z=2,Dc=1.954 g/cm3,F(000)=488,μ =1.353 mm-1,R=0.0248 and wR=0.0761. Complex 2 crystallizes in monoclinic with space group P21/c,a=8.604(3),b=23.88(1),c=8.894(3),β=102.45(1)°,C17H10N4O7Mn,Mr=437.23,V= 1785(1) 3,Z=4,Dc=1.627 g/cm3,F(000)=884,μ=0.791 mm-1,R=0.0471 and wR=0.1250. Complex 1 possesses an infinite 1D polymeric chain structure consisting of the repeated basic four-membered ring units (Cd2O2) and eight-membered ring units (CdOCO)2. Compound 2 displays a linear 1D chain through Mn(Ⅱ) atoms and bridging carboxylate groups of 3,5-dinitrosalicylic acid ligands with the Mn…Mn separation of 4.472(2). The fluorescence properties and cyclic voltammetric behaviors of the complexes are also reported. 相似文献
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The Cluster compound [Cu3BrWOS3(bipy)2] was synthesized by reaction of (NH4)2WOS3, CuBr, 2,2′- bipyridine and n-Bu4NBr at room temperature and characterized by IR, UV and elemental analyses. The structure of [Cu3BrWOS3(bipy)2] was determined by single crystal X-ray diffraction revealing that the cluster consist of a nest -shaped core. The W atom is tetrahedrally coordinated by three S atoms and one O atom. There are two types of copper atoms in the WOS3Cu3 aggregate: two copper atoms are tetrahedrally coordinated and another copper atom is trigonally coordinated. The nonlinear optical properties were studied with an 8ns pulsed laser at 532nm. Its optical responses to the incident light exhibit considerably optical absorptive and strong self-focusing effect with α2=0.90×10-10m·W-1, n2=2.72×10-18m2·W-1. CCDC: 196348. 相似文献
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1 INTRODUCTION There has been extensive interest in manganese complexes containing carboxylate ligands due to the richness in structural chemistry and potential appli- cations in catalysis[1~6], for example, some highly efficient manganese catalysis mimics[7, 8]. Further- more, 4,4?-bipy is an excellent bridging ligand, and so far a number of one-, two- and three-dimensional infinite metal-4,4?-bipy frameworks have already been generated[9, 10]. However, of the above-mentio- ned framework… 相似文献