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1 实 验已有一些用稀土化合物催化Tishchenko和Al dox Tishchenko反应的报道[1~ 4 ] ,本文所用的催化剂对空气和水汽都很敏感 ,所有操作均须用Schlenk技术在氩气保护下进行。溶剂四氢呋喃(THF)和甲苯经无水CaCl2 干燥 ,使用前经二苯甲酮 钠回流至蓝紫色蒸出。丁醛经 0 .4nm分子筛干燥后 ,在氩气保护下蒸出。稀土离子含量用EDTA络合滴定法测定。产物的收率在岛津公司生产的GC 14B型气相色谱仪上测定。1.1 催化剂的合成 (MeCp) 3 Ln由无水LnCl3与MeCpNa按 1∶3摩尔… 相似文献
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2,5-二(2-氨基乙氧甲基)噻吩合成及抑菌活性 总被引:2,自引:0,他引:2
噻吩烷基胺及其衍生物对疟疾、麻风、真菌、病毒和某些肿瘤均有较强的药理活性[1~ 2 ] ,因此合成和开发这类新物质具有重要的意义。以前 ,由 2 噻吩甲醛合成的噻吩类衍生物药物较多[3] ,但对噻吩双取代衍生物的合成研究还未引起重视。因此 ,为了探索这类化合物的性质和抑菌效果。我们合成了未见文献报道的 2 ,5 二 ( 2 氨基乙氧甲基 )噻吩 ,通过多种测试手段 ,确定了它的组成结构 ,其合成路线如下 :1 实验部分1 1 仪器与试剂Nicolet1 70S红外光谱仪 (KBr压片 ) ,PE 2 4 0C型元素分析仪 ,EM 360 60MHz核磁共振仪。… 相似文献
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调吡脲 (Forchlorfenuron ,A) ,代号KT 30 ,化学名N ( 2 氯 4 吡啶基 ) N 苯基脲 ,是一种新型植物生长调节剂 ,具有非常高的细胞激动活性 ,有促进细胞生长、分化作用 ,可以防止植物老化 ,促进苗条形成及果实肥大。对水果果实和烟草叶片等都有促进肥大作用[1 ,2 ] ;对土豆、棉花和甘蔗等农作物也有增产作用。我们参照有关文献[3] 合成了调吡脲 (A)。合成路线如图 1所示。图 1 调吡脲的合成路线Fig .1 Syntheticrouteofforchlorfenuron 合成中 ,吡啶用双氧水进行N 氧化 ,再… 相似文献
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含吡啶环拟除虫菊酯的合成及其杀虫杀螨活性 总被引:5,自引:0,他引:5
在新农药的创制中 ,吡啶作为苯环的生物等排体常被用作分子设计的有效基团 [1,2 ] ,近年来若干含有吡啶环的高效农药如吡虫啉 (Imidacloprid) [3 ] 、盖草能 (Haloxyfop) [4 ] 、啶氧菌酯 (Picoxystrobin) [5]等已被开发应用 .为合成筛选高生物活性化合物 ,我们在前期研究[6 ,7] 的基础上 ,将吡啶环引入拟除虫菊酯的酸部分 ,合成了与戊菊酯 (S- 5 4 3 9) [8] 和氰戊菊酯 (Fenvalerate) [8] 结构相近的新化合物 (5 ,6 ) ,并分离得到化合物 6的两对对映异构体 (α-和β-体 ) .生物活性测试表明 ,这些新化合物具有较高的杀虫或杀螨活性 .目标… 相似文献
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Co(En)3MoO4晶体的水热合成与表征 总被引:1,自引:0,他引:1
杂多酸的水热法合成的深入发展已引起了化学家的广泛关注[1~3].80年代已来,用水热合成方法得到了具有层状[4]、网状[5]、孔道状[6,7]和笼状[8,9]等多种新结构和新组成的杂多酸化合物,并应用于合成药物和研究催化剂等[10,11]工作中.科学家们已深入地了解了钒的氧簇化合物[12~15],但有关钼的氧簇化合物的研究还较少.杨国昱等[16]利用水热法合成了具有孔道结构的Ni(En)3MoO4纳米管.本文在此[16]基础上,利用水热法合成了具有网状结构的Co(En)3MoO4单晶.X射线分析结果表明,该晶体属六方晶系,P3C1空间群,晶体中阴阳离子通过静电吸引作用相互结合,形成一种有机-无机复合材料. 相似文献
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新型化合物[Ni(en)2V6O14]n的水热合成与晶体结构 总被引:1,自引:0,他引:1
金属 -氧簇合物在催化吸附、医药临床、能量存储和材料科学等方面的应用越来越受到关注 [1~ 3 ] .钒 -氧簇合物的结构新颖 ,在材料领域中具有广泛的应用前景 .采用水热合成技术 ,以简单的无机、有机起始原料在相对低温下制备金属 -氧簇合物晶体是近年来刚刚兴起的研究工作 [4 ] ,并且已经合成出一维链状化合物 Cu(prn) 2 V2 O6[5]、层状结构 Ni(C10 H8N2 ) 2 V3 O8.5[6]及三维网状结构 (H2 en Me)[Ni(en) 2 V12 O2 8][7] .我们采用水热技术合成了由 { V V 2 O7} n 单元层与桥配体 [Ni(en) 2 ]2 +构建的三维无机 -有机化合物 [Ni(en… 相似文献
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水热法合成羟基磷灰石的结构和形貌 总被引:2,自引:0,他引:2
羟基磷灰石是一种微溶于水的弱碱性磷酸钙盐 (Ca10 (PO4 ) 6 (OH) 2 ,HA) [1] ,多用于人体硬组织(骨、牙 )的修复替换[2 ] 。与人类骨骼相比 ,致密羟基磷灰石仍然表现出较低的力学性能[3] 。由于针棒状的晶体具有较低的位错密度 ,较高的抗拉性能[4 ] 。近年来 ,针状或棒状羟基磷灰石的合成已引起广泛关注。合成HA的方法有固态反应法[5] 、液相沉淀法[6 ] 、溶胶 凝胶法[7,8] 及溅射法[9] 等 ,但只有少数几种方法能够对产物的形貌进行控制。虽然采用水热法在 2 0 0℃和 2MPa下合成了羟基磷灰石晶须[10 ] ,但实验步骤较为复杂 ,… 相似文献
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We systematically investigated the weak epitaxy growth (WEG) behavior of a series of planar phthalocyanine compounds (MPc), i.e., metal-free phthalocyanine (H2Pc), nickel phthalocyanine (NiPc), copper phthalocyanine (CuPc), zinc phthalocyanine (ZnPc), iron phthalocyanine (FePc), cobalt phthalocyanine (CoPc), grown on a p-sexiphenyl ( p-6P) monolayer film by selected area electron diffraction (SAED) and atomic force microscopy (AFM). Two types of epitaxial relations, named as incommensurate epitaxy and commensurate epitaxy, were identified between phthalocyanine compounds and the substrate of the p-6P film. The tiny variation of the lattice constant of phthalocyanine compounds can result in different crystal orientations. The change rule of incommensurate and commensurate epitaxy was extracted. The tendency of commensurate epitaxy becomes weaker as the lattice constant b increases, while it gets stronger as the substrate temperature is elevated. Large size and continuous H2Pc films can be obtained by controlling the growth conditions. The WEG method is generally applicable in the whole family of planar phthalocyanine compounds and may be used to fabricate other high-quality organic films. 相似文献
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为了确定双核金属酞菁化合物对亚硫酰氯还原反应是否具有比单核金属酞菁更强的电催化性能, 通过循环伏安测试方法, 用酞菁钴和酞菁铁作为对比, 研究了双核钴锰酞菁在1.5 mol·L-1 LiAlCl4/SOCl2电解液中的电催化行为, 并计算出动力学参数, 由此来评估具有平面结构的双核金属酞菁化合物对亚硫酰氯还原的催化活性的影响. 通过比较循环伏安曲线发现, 与单核酞菁钴(II)和酞菁铁(II)相比, 双核钴锰酞菁对SOCl2还原反应具有更好的催化活性, 能提高SOCl2还原反应的交换速率常数和SOCl2在玻碳电极上的扩散系数, 从而提高SOCl2还原电位和电流.通过ER14250型实体电池10 mA放电性能测试验证表明, 与单核酞菁钴和酞菁铁催化剂的电池相比, 双核钴锰酞菁在低温(-30 ℃)下可提高放电中点电压0.3 V, 在常温(25 ℃)下可以提高放电容量约100 mAh, 催化效果比单核酞菁钴和酞菁铁显著. 相似文献
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合成了一种新的α位四戊氧基取代的钯酞菁 ,以其为原料作了不同程度的溴化反应并得到了一系列的酞菁染料溴化物 .实验证明 ,溴化后的酞菁染料最大吸收波长红移 ,摩尔消光系数降低 ,热稳定性也有所降低 ,热失重曲线发生了很大变化 相似文献
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The Influence of the Synthesis Temperature on Cobalt Phthalocyanine Encapsulation in Zeolite Y 总被引:1,自引:0,他引:1
Mohammad Ali Zanjanchi Khalil Tabatabaeian Maryam Moosavifar 《Journal of inclusion phenomena and macrocyclic chemistry》2001,40(3):193-198
Several characterization techniques were applied to study the effect of the synthesis temperature on the physicochemical properties of cobalt phthalocyanine incoporated into zeolite Y. The cobalt phthalocyanine was synthesized in the supercages of zeolite Y by the template synthesis method at two different temperatures of 200 and300 °C and characterized by diffuse reflectance spectroscopy, Fourier transform infraredspectroscopy, pore volume analysis, unit cell dimension calculation, UV-vis spectroscopy,thermogravimetric analysis and X-ray diffraction. The results show that the catalyst synthesizedat 200 °C contains 11 wt.% cobalt phthalocyanine and almost all of thiscomplex is encapsulated in the supercages as monomeric species. At higher temperature aconsiderable amount of the cobalt phthalocyanine is hosted in the mesopores and/or on theexternal surface of the zeolite as aggregates. The migration of one part of the cobalt cationsfrom the supercages to the small cages at 300 °C decreases the formation of thenon-aggregated encapsulated phthalocyanine molecules in the zeolite supercages. Theaggregated cobalt phthalocyanine formed at the surface corresponds to the -polymorph stateof the phthalocyanine. 相似文献
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García-Frutos EM Bottari G Vázquez P Barberá J Torres T 《Chemical communications (Cambridge, England)》2006,(29):3107-3109
An ethynyl-substituted nickel(II) phthalocyanine has been synthesised and its thermotropic properties studied; optical microscopy, differential scanning calorimetry (DSC) and X-ray diffraction (XRD) techniques revealed an unusual mesomorphic behaviour observed for the first time in phthalocyanine systems where each disk of the hexagonal columnar mesophase is formed by two ethynyl-substituted phthalocyanine units. 相似文献
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The phthalocyanine dyes, Remazol Turquoise Blue G133, Everzol Turquoise Blue and Heligon Blue S4 are found to be biosorbed by Phanerochaete chrysosporium (white-rot fungi) and also metabolised by its ligninolytic extracellular enzymes resulting in dye decolourisation, formation of free copper ions and organic metabolites with ultimate extensive phthalocyanine ring breakdown. It is believed that the ligninolytic extracellular enzyme laccase is involved in the early production of a metabolite M8 which involves break-up of the conjugated phthalocyanine ring structure but which retains multi-negative charge. Another ligninolytic extracellular enzyme, manganese peroxidase, is believed to be involved in the release of Cu2+ from the phthalocyanine structure to give a non-copper-containing phthalocyanine metabolite M1 with a slightly longer migration time than the parent dye and absorption at 666 nm. The phthalocyanine ring structure is also broken up by metabolic processes that involve desulphonation and oxidation to give phthalimide (M3) and an unidentified electroactive metabolite M2. Other minor, unidentified metabolites are observed using capillary electrophoresis and liquid chromatography. 相似文献
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Comparison of the photophysics of an aggregating and non-aggregating aluminium phthalocyanine system incorporated into unilamellar vesicles 总被引:2,自引:0,他引:2
The hydrophobic sensitizer, aluminium phthalocyanine chloride (AIPcCI), and the amphiphilic sensitizer, cis-disulphonated aluminium phthalocyanine (cis-AIPcS2), were incorporated into small unilamellar vesicles (SUVs) and large unilamellar vesicles (LUVs). AIPcCI exhibits aggregation, which increases with increasing sensitizer concentration, whereas cis-AlPcS2 is monomeric at all concentrations studied. Complex fluorescence decays are observed, showing decay time distributions which broaden with increasing phthalocyanine concentration. The phthalocyanine aggregate, although non-fluorescent, influences the overall photophysical behaviour of the phthalocyanine-vesicle system. The effect of aggregation on the resulting photophysics of phthalocyanines was investigated by comparing aggregated and non-aggregated phthalocyanine systems. The implications for photodynamic therapy (PDT) are briefly discussed. 相似文献
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Both sequentially deposited double-layered and codeposited composite thin films were prepared by using two kinds of phthalocyanines. The structure and the electrochromic property of these thin films were compared with those of simple phthalocyanine films. The structures of the films were analyzed by scanning electron microscopy (SEM), X-ray diffrction (XRD) and electron spin resonance (ESR) spectra. From the viewpoint of morphology and crystallinity, codeposited thin films have the same structure as the simple one, having sharp peaks at ca. 2θ=7.0° in the XRD pattern and narrow crystal grains in SEM photographs. ESR measurements have revealed that phthalocyanine molecules disperse very well in the codeposited thin films in a molecular level in comparison with the physical mixture of phthalocyanine powders. This high dispersibility of the molecules in the codeposited thin films can play a role to improve the reversibility in the electrochromism. Thus, the reversibility of the phthalocyanine, which shows irreversible electrochromism in the simple film form, can be improved by the codeposition with another phthalocyanine with reversible electrochromism. In contrast, sequentially deposted double-layered thin film gives completely different results. The electrochromism of the double-layered film depends on the property of the simple phthalocyanine thin film which is in contact with the substrate. 相似文献
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本文报道我们合成的几种锌酞菁衍生物在胶束体系中,在电子给体EDTA的存在下,光敏化还原甲基紫精(MV2+)的研究.结果表明,锌酞菁及其衍生物在阳离子表面活性剂的胶束体系中,其敏化效果比在中性或阴离子表面活性剂的胶束体系中更为有效.结构不同的锌酞菁衍生物的敏化效果亦有显著的差异,其中锌酞菁磺酰丁胺敏化效果最好,锌酞菁羧酸次之.用它们作敏化剂时,MV2+形成的量子产率一般高达0.4—0.7,比没有取代基的锌酞菁的敏化效果高. 相似文献
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Thesemiconductivityofphthalocyaninefilmsisstrong1yincreasedinthepresenceofabsorbedelectron-acceptorgas(suchasNO2).ThiseffectsisduetochargetransferbetWeenthee1ectTon-donatingphthalocyaninemoietyandtheelectTon-acceptorgas.ThistopichasbeenstUdiedwidelyinrecentyearswiththeobjectiveofproducinganewgen-erationofgassensors.1-3Here,wereportthepreliminarystUdiesofphotoinduceden-hancementofconductivitychangesinspin-coatedphthalocyaninefilmsexPosedtoNO2gas.Thephthalocyaninefilmswerepreparedbyspin-coat… 相似文献