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1.
氧官能化的膦配体在钯催化的Suzuki-Miyaura反应中的应用   总被引:1,自引:0,他引:1  
合成了带甲氧基和羟基官能团的二茂铁膦配体, 评价了它们在钯催化的Suzuki-Miyaura偶联反应中的性能, 发现带甲氧基的膦配体对钯催化的Suzuki-Miyaura偶联反应有更好的性能, 可催化富电子溴代芳烃和缺电子氯代芳烃与苯硼酸反应高产率地生成相应的联芳烃产物.  相似文献   

2.
谢叶香  王健  李金恒  梁云 《中国化学》2008,26(12):2261-2266
我们发展一种在催化体系可回收和无配体条件下溴化四丁基铵(TBAB)中钯催化卤代芳烃与芳基硼酸的Suzuki-Miyaura交叉偶联反应方法。我们发现水的量对反应有很大的影响。当水的用量为1 %(质量比)时,反应的结果最好。在3 mol%的醋酸钯和1.5 g的TBAB(含1%的水),一系列卤代芳烃与芳基硼酸的顺利地发生Suzuki-Miyaura交叉偶联反应,得到中等及良好的产率。而且在溴代芳烃和活泼的氯代芳烃的交叉反应中,Pd(OAc)2/TBAB催化体系可以回收重复使用多次,并且催化活性基本不变。  相似文献   

3.
钯等过渡金属催化的卤代芳烃和胺的偶联反应   总被引:4,自引:0,他引:4  
张贞发  周伟澄 《有机化学》2002,22(10):685-693
综述了钯等过渡金属催化的卤代芳烃或芳基碘酸酯和胺的偶联反应以及催化这 一新反应的催化剂的发展和应用。用于该反应的配体由P(o-tolyl)3发展到BINAP 及二烷基芳基膦,基底物由溴代芳烃扩展到经济易得的氯化芳烃及碘酸酯和各种胺。  相似文献   

4.
1,3-二烷基咪唑啉/Pd催化卤代芳烃的Heck和Suzuki反应   总被引:1,自引:0,他引:1  
合成并表征了一种新型的有空间需求的N-杂环卡宾前驱体 1,3-二烷基咪唑啉盐. 这些咪唑啉盐与乙酸钯结合形成的高活性催化剂,可在温和条件下催化氯代和溴代芳烃的He ck和Suzuki交叉偶联反应.  相似文献   

5.
张丽园  王磊 《中国化学》2008,26(9):1601-1606
本文报道了有机-无机杂化材料固载的钯催化的无铜Sonogashira偶联反应。在3-[N,N-双(二苯基膦)氨基)]丙基功能化的硅胶固载的钯催化下,末端炔烃和碘代芳烃、溴代芳烃的偶联反应生成高产率相应的偶联产物。反应条件包括使用乙二醇为溶剂,三乙胺为碱。而且硅胶负载的膦钯催化剂和溶剂乙二醇经简单处理,可循环使用6次不降低活性。  相似文献   

6.
溴代烯烃是一类重要的有机合成中间体,通过金属催化的偶联反应可以有效地形成碳-碳及碳-杂键.本文综述了溴代烯烃在金属催化偶联反应中应用的最新进展.  相似文献   

7.
由廉价易得的1,2-环己二胺作为起始原料,通过简单的合成步骤制备了一种新型的四齿膦配体1,并将该配体应用于钯催化的Suzuki交叉偶联反应中.在仅为0.1 mol%的催化剂用量下,成功地实现了多种氯/溴代芳烃、氯/溴代杂环芳烃以及溴代烷烃底物与苯硼酸的交叉偶联反应,产率最高可达99%.  相似文献   

8.
合成了一种新的醚功能化的二茂铁膦3,连到Merrifield树脂上形成负载型的膦配体4;分别开展了膦配体3及其负载型的4在钯催化的Suzuki-Miyaura偶联反应中催化研究;发现相应形成的均相和多相钯催化剂可高产率地催化一系列的溴代芳烃与芳基硼酸偶联形成相应的联芳烃,以及负载型催化剂在不补加钯时具有一定的循环性能.  相似文献   

9.
采在温和条件下羽毛角蛋白负载的Pd纳米颗粒可高效催化水中溴代芳烃与苯硼酸的偶联反应,且具有官能团的广泛适用性,生成的联苯类化合物可在反应液中沉淀出来,具有很好的产率和纯度.催化剂通过简单过滤可重复使用7次.  相似文献   

10.
报道一种在纯水中Pd/C催化的高效Suzuki反应体系,该体系无需除氧,且无外加配体和添加剂,底物普适性广泛,含有亲水或疏水基团的溴代芳烃都能被高效活化. 此外,对部分杂环芳烃与芳基硼酸的偶联反应也有较好的催化效果. 该催化剂可高效循环使用三次,且性能无明显下降.  相似文献   

11.
Phase and structural relationships of the sulfur, selenium, and tellurium compounds of the 4d and 5d transition elements of groups IV to VII of the periodic system are discussed. Homologous elements behave very similarly with respect to the chalcogens, and this is particularly the case for niobium and tantalum, and for molybdenum and tungsten. However, zirconium, niobium, and molybdenum have a greater tendency towards formation of chalcogen-poor phases than their homologues hafnium, tantalum, and tungsten. Subchalcogenides are known only for zirconium and niobium. The number of phases and the tendency towards formation of solid solutions are considerably smaller among the tellurides than among the sulfides and selenides. The crystal structures of the telluride phases also differ from those of the sulfide and selenide phases of analogous composition. In addition, a review of the phase and structural relationships of the arsenic and antimony compounds of the 4d and 5d transition elements of groups V to VII is given.  相似文献   

12.
常温常压下吡咯及其衍生物的镍催化加氢反应考察   总被引:2,自引:0,他引:2  
为进一步研究常温常压下吡咯及其衍生物的镍催化加氢反应,我们对试剂吡咯、吡咯烷和吡咯烷酮做了相应的催化加氢实验。并采用电镜(TEM-HREM)、X射线衍射(XRD)对Ni基催化剂的形貌、结构、加氢活性和超声波对其影响进行了检测,同时还用紫外吸收光谱、气相色谱等对加氢产物进行了分析考察。结果表明超声波能促进镍基催化剂活性,使镍微晶(111)晶面间距增大1.5%、并保持高分散态。常温常压下纳米镍基催化剂对吡咯、吡咯烷和吡咯烷酮的加氢反应显示一定的催化活性;吡咯加氢首先生成吡咯烷,进而使环打开生成低碳烃、氨等产物,总反应为零级,符合表面接触反应特征。  相似文献   

13.
We review the syntheses, optical properties, and biological applications of cadmium selenide (CdSe) and cadmium selenide–zinc sulfide (CdSe–ZnS) quantum dots (QDs) and gold (Au) and silver (Ag) nanoparticles (NPs). Specifically, we selected the syntheses of QDs and Au and Ag NPs in aqueous and organic phases, size- and shape-dependent photoluminescence (PL) of QDs and plasmon of metal NPs, and their bioimaging applications. The PL properties of QDs are discussed with reference to their band gap structure and various electronic transitions, relations of PL and photoactivated PL with surface defects, and blinking of single QDs. Optical properties of Ag and Au NPs are discussed with reference to their size- and shape-dependent surface plasmon bands, electron dynamics and relaxation, and surface-enhanced Raman scattering (SERS). The bioimaging applications are discussed with reference to in vitro and in vivo imaging of live cells, and in vivo imaging of cancers, tumor vasculature, and lymph nodes. Other aspects of the review are in vivo deep tissue imaging, multiphoton excitation, NIR fluorescence and SERS imaging, and toxic effects of NPs and their clearance from the body. Figure Semiconductor quantum dots and metal nanoparticles have extensive applications, e.g., in vitro and in vivo bioimaging Tamitake Itoh and Abdulaziz Anas contributed equally to this article.  相似文献   

14.
纳米材料由于其独特的光、电、磁、力学等性质,成为了构建功能材料与器件的理想基元。实现纳米粒子的精确组装,是探究粒子之间的耦合聚集性质和制备宏观功能器件的基础。但是由于纳米粒子的小尺寸以及在溶液中运动的随机性与复杂性,精准控制纳米粒子组装体的形貌以及在空间中的相对位置仍存在巨大挑战。为了将纳米粒子组装成理想的有序结构,许多控制粒子组装的策略与方法得到发展。本文首先概述了纳米粒子自组装的控制方法与典型形貌,着重分析了影响粒子精准排布的因素与控制方法,并对纳米粒子及其组装体的光学性质与器件应用的最新研究进展进行了讨论,最后对目前纳米粒子精准组装所面临的挑战以及未来发展的方向进行了展望。  相似文献   

15.
基于偶极近似,运用电极化方法,定量研究了电流变液中悬浮颗粒在外电场作用下其体积和形状的变化,并计算了其体积和形状的相对变化率.研究结果表明:悬浮颗粒的体积和形状的相对变化率均与电场强度的平方成正比,并与ER本身的性质有关.一般情况下,颗粒的体积和形状的相对变化率分别为8.4%和12.5%,对总体积变化率的贡献为1.68%.这种变化对于ER系统的电涨和电热都作出了贡献,仅当将颗粒当作刚性球时,其自由能才与电场强度的平方成正比.  相似文献   

16.
Thermal analysis methods are well-established techniques in research laboratories of pharmaceutical industry. The robustness and sensitivity of instrumentation, the introduction of automation and of reliable software according to the industrial needs widened considerably the areas of applications in the last decade. Calibration of instruments and validation of results follow the state of the art of cGMP as for other analytical techniques. Thermal analysis techniques are especially useful for the study of the behavior of the poly-phasic systems drug substances and excipients and find a unique place for new delivery systems. Since change of temperature and moisture occur by processing and storage, changes of the solid state may have a considerable effect on activity, toxicity and stability of compounds. Current requirements of the International Conference of Harmonisation for the characterization and the quantitation of polymorphism in new entities re-enforce the position of thermal analysis techniques. This challenging task needs the use of complementary methods. Combined techniques and microcalorimetry demonstrate their advantages. This article reviews the current use of thermal analysis and combined techniques in research and development and in production. The advantage of commercially coupled techniques to thermogravimetry is emphasized with some examples. This revised version was published online in August 2006 with corrections to the Cover Date.  相似文献   

17.
L—赖氨酸锌细胞生物学和生物学实验研究   总被引:6,自引:3,他引:3  
研究了L-赖氨酸锌对健康大鼠血液及骨髓中细胞的影响,并与对照组进行了比较。结果表明,本品对健康鼠血液中红细胞,血小板,淋巴细胞、中性白细胞和单核细胞及骨髓多染红细胞中的微核数等均无显著性影响,另外大鼠伤寒沙门氏菌的致突变实验显示L-赖氨酸锌未引起大鼠伤寒沙门氏组氨酸缺陷型变异菌株的回复突变,而健康小儿血液各项生化指标的变化,揭示本品可显示提高血液中碱性磷酸酶和红细胞水平,对白细胞的增殖有促进作用,但对乳酸脱氢酶、谷丙转氨酶等无显著性影响。  相似文献   

18.
Unsaturated polyester resin (UPR)/acrylate-terminated polyurethane (ATPU)/organo-modified montmorillonite (OMMT) nanocomposites were prepared by the in situ intercalative polymerization method. Samples were prepared by the sequential mixing, i.e. mixture of the ATPU and styrene (S) and OMMT were prepared in the first step; UPR was then added to the pre-intercalates of ATPU/S/OMMT. Results indicate that the mechanical properties and thermal properties of UPR/ATPU/OMMT nanocomposites greatly depend on the amount of ATPU and OMMT. Results show that the addition of ATPU could increase the impact strength of UPR/ATPU composites, but the tensile strength, flexural strength and heat resistance of the materials are obviously decreased. When the weight ratio between UPR, ATPU and OMMT were 82:15:3, the impact strength and heat distortion-temperature of nanocomposite were greatly improved, meanwhile there was little change for other properties of the nanocomposites. The synergistic enhancement effects of ATPU and OMMT on the composites were observed. The structures and morphology of the composites were investigated by X-ray diffraction, scanning electron microscopy and transmission electron microscopy.  相似文献   

19.
20.
多弧离子镀TiN与不同金属基材间的接触界面与表面特性   总被引:1,自引:0,他引:1  
用多弧离子镀技术在不同金属基材上进行TiN镀膜实验,制备了TiN/Fe、 TiN/Cu和TiN/Cr/Cu复合膜.借助扫描电子显微镜(SEM)、 X射线衍射仪(XRD)和光电子能谱(XPS),研究了TiN与Fe、 Cu和Cr/Cu三种不同衬底接触界面的形貌、结构及其表面特性.SEM观察发现,在一定离子镀膜条件下, TiN涂层可与Fe、 Cu和Cr/Cu金属基材形成均匀平整的接触界面,在铜基上TiN界面清晰,在Fe与Cr/Cu界面有明显的层状晶界微结晶分布.XRD分析显示, Fe、 Cu和Cr/Cu表面生成的薄膜都包含TiN、 Ti2N等多晶相,在Cr/Cu界面还包含Ti-Cr的金属间化合物.XPS结果表明,表面除了TiN膜外,还生成TiO2和TiOxNy等氧化膜.Ar+刻蚀5 min后, TiO2消失, TiOxNy减少, TiN则呈增加趋势.TiN与Cr/Cu界面形成明显的Ti-Cr和Cr-Ni互扩散层,这有助于增强薄膜附着力,形成较牢固的TiN涂层.  相似文献   

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