超声波辐射下合成N-取代苯并噻唑-2-氨基-N'-取代吡唑-4-甲酰基硫脲

为实现多种活性成分的有效叠加和为药物筛选提供先导化合物, 以1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酸为初始原料, 依次合成1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酰氯、1-苯基-3-甲基-5-氯/苯氧基-4-吡唑甲酰基异硫氰酸酯, 再与取代苯并噻唑肼反应生成了8个未见报道的N-取代苯并噻唑-2-氨基-N'-取代吡唑-4-甲酰基硫脲. 采用超声波催化法合成了标题化合物, 并与加热回流的常规方法进行了对比. 超声波催化法具有操作简单、反应时间短、条件温和、产率高、副反应少等优点, 为此类化合物的合成提供了一种有效的新方法. 标题化合物经元素分析, IR, ¹H NMR确证结构.     

多步法制备纳米钛酸钡

采用醋酸钡、碳酸钾、钛酸丁酯等为初始反应物，通过多步反应的方法，制得了纳米钛酸钡。所得产品采用XRD、TEM和SEM等进行了表征，并对生长机理进行了分析。研究结果表明，得到的碳酸钡为直径约100 nm的纳米棒，再经室温下钛酸丁酯水解产生二氧化钛对碳酸钡纳米棒进行包覆，可得到一维核-壳结构的碳酸钡/二氧化钛，最后于700 ℃下经固相反应而得到钛酸钡的纳米颗粒。这种制备纳米钛酸钡的方法可以有效地控制产品形貌及粒径。     

Synthesis, Structure and Characterization of a Novel Asymmetrical Half-sandwich Binuclear Iron Carborane Complex [η~5-C_5H_3(t-Bu)_2]_2Fe_2(CO)_3Se_2C_2B_(10)H_(10)

IntroductionThe chemistry of chalcogen organometalliccomplexs has become one of the most activebranches in modern chemistry[1] .Itnot only showsthe coordinate variability of organometalliccomplexes but also is applied to studying thereaction mechanism of biologic enzyme[2 ] and thecatalysis of dehydrogenation or hydrogenation inindustry[3] .It is known that transition metalcomplexes react with cyclopentadienyl orsubstituted cyclopentadienyl to form halfsandwichcomplexes with different structur…     

Synthesis and X-ray crystal structure of oxamido-bridged heterobinuclear Ni(Ⅱ)-Cu(Ⅱ) complexes

The two complexes [Ni(oxen)Cu(L)2](ClO4)2.xH2O (L=2,2'-bipyridyl(bpy), 1,10-phenanthroline(phen)) have been synthesized, where oxen is N,N'-bis(2-aminoethyl)oxamido di-anion. The crystal structure of [Ni(oxen)Cu(bpy)2](ClO4)2.CH3OH has been determined by X-ray diffraction method. The crystal is triclinic system, space group P1 with a=12.179(1),b=12.298(2), c=11.476(2) A, a=97.57(1), B=97.52(1), 7=80.29(2), V=1669.04(67) A3, Z=2, Dcalcd=1.667 g/cm3. The structure has been refined to final R of 0.076 and Rw of 0.080, respectively. The complexes have an extended oxamido-bridged structure and consist of Ni(Ⅱ) ion in a square planar environment and Cu(Ⅱ) ion in a distorted octahedral environment.     

Effect of Variant Counterions on Stability and Particle Size of Silica Sol

The effects of variant counterions with ionic strength of 0.05, 0.10, 0.20 and 0.25 mol·kg^-1 on the stability and particle size of silica sols have been studied using the traditional methods of Ubbelohde viscosity measurement, TEM and titration respectively, finding that the stability and particle size of the silica sols are all concerned with the acidic, positively electric properties and the sizes of the counterions, as well as the attraction between the counterions and surface silicon hydroxyl groups of the silica sols. The small positively charged counterions lead to the decrease in particle sizes, making the silica sol the most stable. But the larger weakly acidic counterions can restrict the particle sizes of the silica sols and easily make the sols coagulate. It was also found that there existed a linear relationship between log r and log η, which has not ever been reported. The effect of temperature on the stability and particle sizes was also discussed.     

锂离子电池正极材料LiMn2O4的低热固相合成与性能表征

锂离子电池具有比能量高、环境污染小等优点,广泛应用于手提电话、便携式电脑、摄像机等设备中。其正极材料的研究是锂离子电池的研究重点。层状结构的LiCoO2、LiNiO2和尖晶石结构的LiMn2O4是仅有的三种能在3.5V以上电位可嵌入Li的正极材料[1~3]。目前市售的锂离子电池主要采用LiCoO2作正极材料,但由于Co资源缺乏和价格相对昂贵,而锰资源丰富,价格低廉且无毒,对环境友好,因此世界各国都在大力进行以LiMn2O4为正极材料的锂离子电池的实用化研究。LiMn2O4传统的制备方法是高温固相反应合成法[4~7],但由于Mn的变价多,与Li形成贫Li或…     

基于芳香四羧酸构筑的两种配位聚合物的荧光及磁性质（英文）

在溶剂热条件下,基于芳香四羧酸合成了2种新颖的配位聚合物:{[Zn2(tptc)(1,4-bimb)2]·H2O}n(1)和{[Ni(tptc)0.5(1,2-bimb)(H2O)]·H2O}n(2),其中,tptc为对-三联苯-3,3″,5,5″-四羧酸,1,4-bimb为1,4-二(咪唑-1-亚甲基)苯,1,2-bimb为1,2-二(咪唑-1-亚甲基)苯。结构分析表明,1为三维结构,拓扑符号为(86);2为二维层状网络,通过氢键相互作用进一步扩展为三维超分子结构。此外,我们还研究了1对阳离子、阴离子的荧光感应以及2的磁性质。     

环氧化橡胶及其合金的研究与应用

综述了国内外环氧化橡胶及其合金的研究现状和应用趋势,重点介绍了环氧化天然橡胶、环氧化聚丁二烯、环氧化苯乙烯-丁二烯-苯乙烯三嵌段共聚物及其合金的优点,以及影响其物理机械性能的因素和环氧化橡胶的发展方向。     

GAS SORPTION AND TRANSPORT IN POLY (PHENYLENE OXIDE)(PPO)AND ARYL-BROMINATED PPO MEMBRANES

The apparent solubility (S), concentration-average diffusivity (D), and permeability (P), for C0_2, CH_4 and N_2 through PPO and aryl-brominated PPO at 35℃for pressure ranging from 1 to 26 atm are reported. It is found that P, D, and S of the membranes to all the three gases vary with the extent of bromination. S increases with the increase of the percent of bromine in each case, but D to CO_2 increases remarkably only at higher degree of brominafion, and therefore, P to CO_2 is increased by more than 100% over a wide range ofpressure in the case. The solubility data are well described by the dual mode sorption model. It is found that the gas molecules sorbed by the Langmuir mode are relatively more immobilized and the contribution of the nonequilibrinm character of the polymer to gas permeation increases obviously for CO_2 and is hardly changed for CH_4 with increasing bromine content. These observations are interpreted in terms of changes in specific free volume (SFV)and the cohesive energy density (CED) of the polymers.     

肽核酸骨架分子键联卟啉的合成及结构表征

以5,10,15-三苯基-20-(4-羧基苯基)卟啉和5,10,15-三苯基-20-(4-羟基苯基)卟啉为原料, 分别与N-(Boc-氨乙基)甘氨酸乙酯(3)及其衍生物4作用, 得到了两种肽核酸骨架分子键联卟啉化合物6和8. 中间体和目标化合物均由紫外-可见光谱、红外光谱、核磁共振光谱、质谱及元素分析所确证. 目标化合物的荧光光谱测试结果表明, 肽核酸单元分子的链接对卟啉分子的荧光波长和强度影响不大.