新型六氢吡啶-2,3-并吲哚化合物的合成及其抗肿瘤活性

以3-取代氧化吲哚与丙烯酸酯为原料,经Michael加成反应制得中间体--3-丙酸酯取代氧化吲哚（3a~3d）; 3a~3d与甲胺发生酰胺化反应制得3 丙酰胺取代氧化吲哚（4a~4d）; 4a~4d用氢化铝锂还原-环化,合成了4个六氢吡啶-2,3-并吲哚化合物(5a~5d）; 5a和5b用氢化铝锂还原合成了2个六氢吡啶-2,3-并吲哚化合物（6a和6b）, 5a～5d, 6a和6b均为新化合物,总产率42%～61%,其结构经¹H NMR, ¹³C NMR和HR-ESI-MS表征。采用MTT法研究了5a～5d, 6a和6b对人肺癌细胞（A549）,人前列腺（PC-3）和人白血病细胞（K562）的体外抗肿瘤活性。结果表明：5b对A549, PC 3和K562的抑制活性均较好,其IC₅₀分别为27.2μmol·L^-1, 37.5 μmol·L^-1和21.7 μmol·L^-1。     

Cu/MgO催化剂的MOCVD法制备及其γ-戊内酯加氢制1,4-戊二醇性能

以Cu（acac）₂为金属有机铜前体,层状MgO为载体,采用金属有机化学气相沉积方法（MOCVD）制备了Cu/MgO催化剂,并通过X射线衍射（XRD）、傅里叶变换红外光谱（FT-IR）、场发射扫描电镜（FE-SEM）、透射电子显微镜（TEM）和N₂物理吸附等方法对Cu/MgO催化剂结构进行表征。结果表明,有机铜前体沉积在了MgO上,并且在沉积后,载体MgO的晶体结构仍然保留完整。利用生物质平台分子γ-戊内酯加氢反应来评价Cu/MgO催化剂的催化性能。研究表明,在473 K和10 MPa反应条件下,18% Cu/MgO催化剂表现出优异的催化活性（90.5%）和1,4-戊二醇选择性（94.4%）,且催化剂循环三次,催化活性没有显著降低。     

碳点的性质及其在化学发光分析中的研究进展

碳点是一种新型的荧光碳纳米颗粒,与传统的半导体量子点相比,碳点具有毒性低、生物相容性好、原料丰富廉价、光稳定性好等特点,得到引了化学、材料和生物等各领域科学家的高度关注。 本文介绍了碳点的基本概念和性质、探讨了碳点在化学发光领域的应用研究进展并进行了展望。     

Synthesis,Crystal Structure and Antitumor Activity of Tectochrysin-6-sulfonate

In order to enhance water-solubility and biological utilization rate of tectochrysin,sodium 5-hydroxyl-7-methoxyflavone-6-sulfonate(1) was synthesized and its structure was identified on the basis of 1 H NMR,FT-IR and elemental analysis.5-Hydroxyl-7-methoxyflavone-6-sulfonate was assembled with Ni(II) or Mn(II),hexaquanickel(II) bis(5-hydroxyl-7-methoxyflavone-6-sulfonate) tetrahydrate(2) and hexaquamanganese(II) bis(5-hydroxyl-7-methoxyflavone-6-sulfonate) tetrahydrate(3) were obtained and characterized by IR spectroscopy.The crystal structures of 2 and 3 were determined by X-ray single-crystal diffraction analysis.The results showed that 2 and 3 are isomorphous crystals and crystallize in monoclinic crystal system,space group C2/c.In 2 and 3,the supramolecular structures are organized into hydrophilic and hydrophobic regions.Hydrophilic regions are generated by O–H???O hydrogen bonds among sulfonate groups,latticed water molecules and coordinated water molecules.The π-π stacking interactions assemble the flavone skeletons into columns and these columns form hydrophobic regions.The sulfonate groups play an important role as a bridge of the hydrophilic and hydrophobic regions as well as the inorganic and organic components.Three-dimensional networks of 2 and 3 are furnished by extensive array of hydrogen bonds,π-π stacking interactions and electrostatic interactions.The anti-proliferative activities of 1~3 in vitro against human leukemia cells K562 and human lung cancer cells A549 were evaluated by the standard MTT assay.The pharmacological activity results showed that the introduction of sulfonic acid groups enhanced the antitumor activity of tectochrysin.     

一例钴基金属有机框架化合物活化过氧单硫酸盐高效降解水中亚甲基蓝研究

在水净化领域,基于硫酸根自由基(SO₄^·-)的高级氧化工艺因其高选择性和氧化优势应用潜力巨大.开发高性能过氧单硫酸盐(PMS)催化剂是染料废水处理的研究热点.此工作中,选用5,5’-二苯醚间苯二甲酸(H₄odip)和Co²⁺离子通过溶剂热法合成得到一例新的钴基金属有机框架化合物Co(μ₆-odip)_0.5(μ₂-OH₂)_0.5(H₂O)₂·1.5H₂O (1).该化合物水稳定性和热稳定性优良且具有一定的耐酸碱性.通过X-射线单晶和粉末衍射、热重分析、元素分析和红外光谱表征了该化合物的结构及组成.化合物1属于单斜晶系C2/c空间群,晶胞参数为a=1.6101(9) nm,b=1.5508(10) nm,c=0.9660(6)nm,α=90°,β=112.70(2)°,γ=90°.通过紫外-可见分光光度计对1活化过氧单硫酸盐降解水...     

石墨烯量子点功能化金纳米粒子的制备及作为过氧化物模拟酶用于葡萄糖检测

基于石墨烯量子点（GQD）的还原性,在无需外加保护剂的条件下,采用一步法成功制备了稳定性高、分散性好的石墨烯量子点功能化的金纳米粒子（GQD@AuNPs）.所制备的GQD@AuNPs有优良的过氧化物模拟酶催化活性,能够有效地催化H₂O₂氧化3,3’,5,5’-四甲基联苯胺（TMB）产生显色反应.以TMB为模型底物,研究了催化条件（温度和pH）对催化活性的影响.电子自旋共振光谱（ESR）结果表明,GQD@AuNPs与辣根过氧化物酶（HRP）类似,能有效地催化H₂O₂分解成羟基自由基（^·OH）.基于此,结合葡萄糖在葡萄糖氧化酶（GOx）作用下产生H₂O₂的原理,建立了可视化检测血清中葡萄糖含量的简便方法.在优化条件下,本方法的检测范围为2.0×l0^-6～4.0×l0^-5 mol·L^-1,检出限为3.0×l0^-7 mol·L^-1,并对实际样品进行测定,测定结果与临床结果一致.     

Synthesis,Crystal Structure and Antineoplasmic Activity of 3,6,8-Tribromo-5-hydroxy-2,7-dimethoxy-2-phenyl-2,3-dihydrochromen-4-one

The reaction of 5-hydroxyl-7-methoxyflavone(tectochrysin) with bromine obtained 3,6,8-tribromo-5-hydroxy-2,7-dimethoxy-2,3-dihydrochromen-4-one(1), which was characterized by FT-IR, 1 H-NMR, ~(13)C-NMR, elemental analysis and X-ray single-crystal diffraction. Complex 1 belongs to the monoclinic system, space group pbca with a = 9.4673(8), b = 17.9938(15), c = 21.2004(17) ?, V = 3611.5(5) ?~3, Z = 8, μ = 0.6726 mm~(-1), Dc = 1.795 g/cm3, F(000) = 2080, the final R = 0.0358 and wR = 0.0644 with I 2σ(I). The results show that the addition reaction occurs at the carbon-carbon double bond(C2 and C3) of tectochrysin and 1 belongs to dihydroflavone. The reaction mechanism was discussed and the structure revealed that the crystal structure of 1 is stabilized by intramolecular hydrogen bonds and C–Br···π interactions. The antitumor ability of 1 was evaluated against human leukemia cells(K562), human breast cancer cells(MCF-7) and human lung cancer cells(A549). 1 exhibited potent antitumor activities against human leukemia cells(K562) with the IC50 values of 18.9 μmol/L.     

钛基固体超强酸对环己酮乙二醇缩酮催化反应的特性

合成S042-/TiO2、SO42-/TiO2-Ce(Ⅳ)、SO42-/TiO2-ZrO2三种不同的固体超强酸,以环己酮乙二醇缩酮为探针反应,发现550℃下焙烧的SO4 2-/TiO2-Ce(Ⅳ)催化活性最好.并以SO42-/TiO2-Ce(Ⅳ)为催化剂,考察反应温度、催化剂用量、反应时间、反应物配比和带水剂对缩酮化反应转化率和选择性的影响.结果表明,反应温度为110～125℃、催化剂用量占反应物料总质量的0.5%、环己酮和乙二醇物质的量比为1:1.5、反应时间为1 h、环己烷为带水剂时,环己酮的转化率达95.2%,环己酮乙二醇缩酮的选择性98.7%,催化剂的重复使用效果好.