氯化铜催化偶联合成4-烷基联苯

4-烷基联苯是重要的液晶中间体. 以氯化铜为C—C键偶联反应催化剂, 经过对溴联苯的Grignard试剂直接与溴代烷烃发生偶联反应, 成功合成了一系列4-烷基联苯类化合物, 部分化合物产率高达91%左右, 并对其反应条件进行了初步研究; 所合成化合物结构都经过元素分析、红外光谱、核磁共振氢谱和质谱鉴定. 与现有方法相比, 此合成方法收率高、环境友好、成本相对较低.     

Synthesis and Quantum-chemistry Analysis on Novel Triazole Compounds Containing Ester Group

Nine novel triazole compounds containing ester group were designed and synthesized. Their structures were confirmed by elemental, ^1H NMR and IR analyses, and optimized by means of DFF （Density Functional Theory） method at the B3LYP/6-31G＊ level. Based on the quantum-chemical calculation results and the Pearson coefficients between FA and quantum- chemical parameters, V, LogP, MR and EHOMO are shown to be the important relative factors which affect FA of the title compounds.     

A Chain Structure Based on Homodinuclear Scandium Units： [Sc（μ-OH）（2,5-pydc）（H2O）]n

The reaction of pyridine-2,5-dicarboxylic acid with Sc2O3 under hydrothermal con- dition yields a new complex [Sc（μ-OH）（2,5-pydc）（H2O）]n 1 which has a chain structure based on homodinuclear scandium units. Crystal data for 1： space group P^-1, a = 6.7192（13）, b = 7.6131（13）, c = 8.9313（14） A, α = 95.976（6）, β = 101.663（6）, γ = 108.151（5）^o, V= 418.26（13） A^3, Z = 2, Dc = 1.946 g/cm^3, g = 0.889 mm^-1, F（000） = 248, C7H6NO6Sc, Mr = 245.09, the final R = 0.0429 and wR = 0.1086.     

Synthesis and Crystal Structure of a Novel Tetranuclear Complex [Pb4（HQ）6（NO3）2]

Reaction of 8-hydroxyquinoline （HQ） with Pb（NO3）2 in water resulted in the formation of a tetranuclear complex [Pb4（HQ）6（NO3）2] 1. It has been characterized by IR, elemental analyses and X-ray diffraction. Crystal data for this complex： triclinic system, space group P1, a = 9.7399（6）, b = 11.6535（8）, c = 12.6806（8） A, α = 62.8050（10）, β = 78.4910（10）, γ = 80.5490（10）°, C54H36N8O12Pb4, Mr= 1817.67, Z = 1, V = 1250.04（14）A^3, Dc = 2.415 g/cm^3,μ = 13.503 mm^-1, -12≤h≤8, -14≤k≤13, -15≤1≤15, F（000） = 840, Rint = 0.0217, R= 0.0348 and wR = 0.0927. X-ray crystal structure analysis revealed that in 1 each Pb（ II ） contains a stereo- chemically active lone pair of electrons. The Pb…C interaction, C-H……O weak interaction and π…π stacking interactions are observed in the complex. In the solid state, the complex possesses strong photoluminescent emission at 485 and 528 nm.     

卟啉修饰g-C3N4提高光催化产氢活性研究

半导体光催化制氢是一种可实现持续制备和储存氢气的绿色技术.石墨相氮化碳(g-C3N4)是研究广泛的光催化剂,但其仍存在光利用率低、光生电子和空穴易复合等问题,制约着光催化产氢的性能.利用给电子卟啉修饰g-C3N4,构建了四(4-羧基)苯基卟啉(TCPP)以共价/非共价方式修饰g-C3N4的催化剂.卟啉共价修饰g-C3N4(gC3N4-TCPP0.1)及非共价复合结构(TCPP0.1/g-C3N4)光催化产氢速率分别为6 997和5 399μmol·g-1·h-1,较g-C3N4分别提高了53%和18%. TCPPx/g-C3N4异质结加强了界面接触,促进了电荷转移,增强了可见光吸收能力,进而提高了光催化制氢性能. g-C3N4-TCPPx中, TCPP的接枝拓展了共轭结构,优化了电子结构,增大了分子偶极,促进了电荷分离,共价桥键为电荷传输提供了通道.     

Organic Memristor Based on High Planar Cyanostilbene/Polymer Composite Films

Organic memristors with low power consumption, fast write/erasure speed, and complementary metal-oxide-semiconductor(CMOS) compatibility have attracted tremendous attention to mimic biological synapses to realize neuromorphic computation in recent years. In this paper, organic resistive switching memory(ORSM) based on (Z)-3-(naphthalen-2-yl)-2-(4-nitrophenyl)acrylonitrile(NNA) and polymer poly(N-vinylcarbazole)(PVK) composite film was prepared by spin-coating method. Device performance based on NNA:PVK composite films with different mass fractions of NNA were systematically investigated. The ORSM based on PVK:40%(mass fraction) NNA composite film exhibited non-volatile and bipolar memory properties with a switching ratio(I_on/I_off) of 24.1, endurance of 68 times and retention time of 10⁴ s, a “SET” voltage(V_set) of -0.55 V and a “RESET” voltage(V_reset) of 2.35 V. The resistive switching was ascribed to the filling and vacant process of the charge traps induced by NNA and the inherent traps in PVK bulk. The holes trapping and de-trapping process occurred when the device was applied with a negative or positive bias, which caused the transforming of the conductive way of charges, that is the resistive behaviors in the macroscopic. This study provides a promising platform for the fabrication of ORSM with high performance.     

8-羟基喹啉共轭连接芳香杂环化合物的合成、荧光性质及生物活性的研究

设计合成了4个8-羟基喹啉共轭联接芳香杂环化合物来研究它们在有机发光材料和荧光探针的潜在应用。用IR, 1H NMR, 13C NMR, MS, UV确认了这些新化合物的结构。测定了化合物1-4的荧光性质,发光衰变时间和量子产率,并用密度泛函方法研究了4个化合物的几何结构和荧光发射波长的关系。在调控骨髓间充质干细胞增殖以及清除DPPH自由基的活性测试结果表明,这些化合物具有促进小鼠骨髓间充质干细胞的增殖的活性及良好的抗氧化性。     

伊维菌素缓释微球片剂的体外释放评价

【目的】研究不同缓冲体系对以玉米醇溶蛋白为载体制备的具有缓释性能的伊维菌素微球片剂药物溶出速度的影响;【方法】体外模拟大鼠胃肠道环境,测定伊维菌素微球片剂在不同缓冲体系中药物溶出以及释放动力学;【结果】在0.1mol/LHCl和磷酸氢二钠-柠檬酸缓冲液(pH=2.2)中,2h药物溶出率分别为19.60±0.95%和25.62±5.17%(p>0.05);在0.1mol/LHCl 0.32%胃蛋白酶(w/v)、磷酸氢二钠-柠檬酸缓冲液(pH=2.2) 0.075%胃蛋白酶(w/v)和磷酸氢二钠-柠檬酸缓冲液(pH=2.2) 0.0375%胃蛋白酶(w/v)中,2h药物溶出率分别为62.00±3.76%、74.18±8.26%和64.61±3.20%;在含有大鼠5%胃内容物的0.1mol/LHCl体系中,IVM在2h内溶出的百分率为42.27%,然后转移到含有大鼠4%小肠内容物的PBS体系中继续溶出3h,溶出百分率为88.03%;【结论】胃蛋白酶可以加速伊维菌素从微球片剂中的溶出。     

纳米硫化铜颗粒自组装为球、空心球和线形结构

用水和乙二醇混合物为溶剂,应用溶剂热合成方法制备了由纳米颗粒自组装的球、空心球和线形结构的铜的硫化物,如 Cu7S4, Cu1.8S, Cu1.81S 和 Cu2S。 考查了溶剂组成（水含量的变化）、反应时间、实验温度的变化对所制备样品的形貌和物相结构的影响。研究了其形成机理。结果表明,随着反应时间的变化,首先形成纳米颗粒的铜的硫化物。通过自组装形成线形结构。最后转化为球形或空心球形结构。     

酰氨基硫脲类新型分子钳受体的合成及其对氟离子的识别性能研究

本文设计并高产率合成了三种新型阴离子识别受体化合物,它们对F-的识别选择性较卤素其他阴离子的高。其对F-的识别性能通过紫外—可见光谱和核磁共振氢谱进行了检测,光谱数据表明,在DMSO溶液中受体与F-通过氢键相互作用形成1:1配合物。与以前我们报道的受体化合物相比,由于此类分子钳受体化合物具有更多的阴离子识别位点,因此具有更好地阴离子识别性能。