苯萘基糖苷类化合物的合成及其治疗糖尿病的活性

以1,2-二甲氧基苯,丁二酸酐以及α-溴代四乙酰基吡喃糖为原料,设计并合成了作为SGLT2抑制剂的两个结构新颖的苯萘基糖苷化合物(6a和6b),其结构经1H NMR, 13C NMR, IR和ESI-MS确认.利用小鼠体内葡萄糖耐受量法测定了6治疗糖尿病的活性,结果发现6a具有明显的降血糖作用,其活性与阳性对照药格列齐特相当.     

新型苯基噻吩-2-基甲酮类化合物的合成及其对人脐静脉内皮细胞的保护活性

合成了13个具有新型结构的苯基(噻吩-2-基)甲酮类化合物,其中3个化合物(9b,10b,11b)未见文献报道,目标化合物的结构均经ESI-MS、1H NMR和13C NMR等技术手段进行了确证。 对H2O2诱导的人脐静脉内皮细胞(HUVECs)氧化损伤保护活性的结果显示,对位甲氧基以及两个氯原子取代的活性较好。 初步构效关系表明,苯基噻吩甲酮母环上取代基的位置、数目、类型是影响化合物活性的主要原因。     

新型蒎烷基噻唑衍生物的合成及其生物活性研究

以β-蒎烯的衍生物诺蒎酮为原料,合成了系列新型蒎烷基噻唑衍生物,并对其生物活性进行了研究.β-蒎烯经高锰酸钾氧化所得到的诺蒎酮与氨基硫脲进行缩合反应,得到诺蒎酮缩氨基硫脲;诺蒎酮缩氨基硫脲再与α-卤代酮进行环化,得到新型蒎烷基噻唑衍生物2a~2l.采用FTIR,1H NMR,13C NMR和HRMS对化合物2a~2l的结构进行了表征.探讨了化合物2a~2l的抑菌活性、对人脐静脉内皮细胞(HUVECs)的抗炎活性以及对紫薇蚜虫的杀虫活性.结果表明,化合物2b具有很好的抗菌活性,对细菌和真菌的抑制效果分别与阿米卡星和酮康唑的效果相当;化合物2a则具有显著的抗炎活性,化合物2e、2h、2i和2k对紫薇蚜虫具有一定的杀虫活性.     

新型吡唑硫代酰胺衍生物的合成

首次合成了7个新的5-(2-羟基-6-甲氧基苯基)-3-甲基-N-取代酰基-4,5-二氢吡唑-1-硫代酰胺衍生物,其结构经1H NMR,IR和元素分析表征。初步生物活性测试结果表明,部分化合物具有杀菌活性。     

新型N-酰基-7-甲氧基-苯并[4,5]噻唑并[2,3-c][1,2,4]三唑-3(2H)-硫酮的合成及其除草活性

为了寻找新的含苯并噻唑稠杂环农药先导化合物,以2-氨基-6-甲氧基苯并噻唑为起始原料,经肼化、环化和酰基化反应,合成出了14个N-酰基-7-甲氧基苯并[4,5]噻唑并[2,3-c][1,2,4]三唑-3(2H)-硫酮,并利用1H NMR,ESI-MS及元素分析对其结构进行表征.对目标化合物进行初步的除草活性筛选,实验结果表明:在浓度为200 mg/L时,大部分化合物对黄瓜(Cucumis sativus)、小麦(Triticum aestivum)、高粱(Sorghum vulgare)、萝卜(Raphanus sativus)、油菜(Brassica campestris)和稗草(Echinochloa crusgalli)的根和茎的抑制率在85%以上.     

4,6-二氯-5-(2-甲氧基苯氧基)-2,2'-联嘧啶的合成

以丙二酸二乙酯为原料,经溴化、醚化得甲氧基苯氧基丙二酸二乙酯(3);3与嘧啶甲脒环合、卤代合成了4,6-二氯-5-(2-甲氧基-苯氧基)-2,2'-联嘧啶,总收率37.29%,其结构经1H NMR,IR和MS确证。     

4,6-二氯-5-(2-甲氧基苯氧基)-2,2′-联嘧啶的合成

以丙二酸二乙酯为原料,经溴化、醚化得甲氧基苯氧基丙二酸二乙酯(3);3与嘧啶甲脒环合、卤代合成了4,6-二氯-5-(2-甲氧基-苯氧基)-2,2′-联嘧啶,总收率37.29％,其结构经1H NMR,IR和MS确证.     

含有2,4-二卤代联苯基的新型唑类衍生物的合成及其抗真菌活性

以2,4-二卤代联苯为原料,经傅-克酰基化、还原、取代等反应步骤,合成了含有2,4-二卤代联苯基的新型唑类目标化合物3a~3k,其结构用红外光谱(IR)、高分辨质谱(HMRS)、核磁共振氢谱(¹H NMR)、核磁共振碳谱(¹³C NMR)等技术手段进行了表征。 测试了目标化合物的体外抗真菌活性,结果表明,所有目标化合物对所测试的致病真菌均有一定程度的抗真菌活性。 其中化合物3a~3k对红色发癣菌和石膏样毛癣菌的抗真菌活性和两性霉素B相当,化合物3b、3c、3e、3f、3h、3i、3k对白色念珠菌的抗真菌活性优于或等于酮康唑。     

高纯度(>98%)三芳基-2-硼酸的合成

以卤代芳烃为原料,经硼酸化反应和Suzuki偶联反应合成了一系列三芳基-2-硼酸化合物,收率67.4%~70.1%,纯度均98%,其结构经1H NMR和元素分析确证。     

6-溴(氯)-2-氯甲基-3-喹啉甲酸乙酯的合成方法研究

以邻硝基苯甲醛为起始原料,经还原和氨基保护合成2-乙酰胺基苯甲醛(1)。应用环境友好的聚乙二醇-400为溶剂,以N-卤代丁二酰亚胺为卤代试剂对化合物2-乙酰胺基苯甲醛(1)进行卤代,制备了5-溴(氯)-2-乙酰胺基苯甲醛(2a,2b)。在三甲基氯硅烷(TMSCl)催化作用下,5-溴(氯)-2-乙酰胺基苯甲醛(2a,2b)与4-氯乙酰乙酸乙酯发生Friedlnder缩合反应,合成目标产物6-溴(氯)-2-氯甲基-3-喹啉甲酸乙酯(3a,3b)。其中2a,2b,3a,3b的结构经IR、1H NMR、13C NMR、MS得以确定。     

KCl-KBO2-K2CO3, K2MoO4-KBO2-K2CO3, and K2WO4-KBO2-K2CO3 ternary systems

phase diagrams of KCl-KBO₂-K₂CO₃, K₂MoO₄-KBO₂-K₂CO₃, and K₂WO₄-KBO₂-K₂CO₃ ternary systems were studied by a calculation-experimental method and differential thermal analysis (DTA). The coordinates of ternary eutectics were determined to be E ₁: 622°C, 8.5 mol % KBO₂, 56.5 mol % KCl, and 35 mol % K₂CO₃; E ₂: 710°C, 23 mol % KBO₂, 43 mol % K₂CO₃, and 34 mol % K₂MoO₄; E ₃: 710°C, 23 mol % KBO₂, 43 mol % K₂CO₃, and 34 mol % K₂WO₄. The specific heats of melting of the eutectics were determined.     

Solubility in the Na2Cr2O7-(NH4)2Cr2O7-K2Cr2O7-H2O system

Solubility in the Na₂Cr₂O₇-(NH₄)₂Cr₂O₇-K₂Cr₂O₇-H₂O four-component water-salt system at 25, 50, and 75°C was studied for the first time. Phase field boundaries for individual salts and potassium and ammonium dichromate solid solutions, monovariant lines, and invariant points were determined. Experimental data were used to optimize the looped isohydric process of potassium dichromate preparation involving additional salts.     

Li2O-TiO2-SiO2-P2O5和Li2O-TiO2-Al2O3-P2O5体系锂离子固体电解质的制备及性能研究

一些具有NASICON型网格结构的固体电解质具有高的电导率和好的稳定性,NASICON的意思是Na Super Ionic Conductor[1]。当NaZr2(PO4)3中P5 被Si4 部分取代时便可以得到具有NASICON结构的Na1 xZr2SixP3-xO12体系,其具有高的钠离子电导率。然而有相同结构的Li1 xZr2SixP3-xO12体系的离子电导率却很低,这是因为Li 半径太小,而NASICON三维网格结构的离子通道太大,两者不匹配而使电导率下降[2]。但当LiZr2(PO4)3中Zr4 被离子半径小些的Ti4 取代,所得LiTi2(PO4)3的通道就与Li 半径相匹配,适合于锂离子的迁移,从而使其电导率…     

Li2SO4-Na2SO4-H2O和Li2SO4- K2SO4-H2O溶液的体积性质

本文用高精度数字式振荡管密度计测定了288K至318K温度范围内Li₂SO₄ + Na₂SO₄ + H₂O和 Li₂SO₄ + K₂SO₄ + H₂O三元体系的密度。混合溶液的离子强度范围从0.1到4.5 mol.kg_–1,混合溶液中Na₂SO₄和K₂SO₄的离子强度分数为0.2,0.4,0.6和0.8。用密度实验值拟合得到了不同温度下Pitzer离子相互作用模型混合参数θ_V和 ψ_V,模型的计算值与实验值的偏差在±0.002 g.cm_–3以内。用Pitzer模型计算了不同离子强度下三元体系的混合体积。     

The preparation of NbH5(Me2PCH2CH2Me2)2 and NbHL2(Me2PCH2CH2PMe2)2 (L = CO or C2H4)

MMe₅(dmpe) (M = Nb or Ta, dmpe = Me₂PCH₂CH₂PMe₂) reacts with H₂ (500 atm) and dmpe in THF at 60°C to give MH₅(dmpe)_2? NbH₅(dmpe)₂ readily reacts with two mol of CO or ethylene (L) to give NbHL₂(dmpe)₂. The exchange of the hydride ligand with the ethylene protons in NbH(C₂H₄)₂(dmpe)₂ is not rapid on the ¹H NMR time scale (60 MHz) at 95°C.     

(H2NC4H8NCH2CH2NH2)(HNCH2CH2NH2)3Zn2Ge2Se8: A new,templated one-dimensional ternary semiconductor stabilized by mixed organic cations

The novel, 1D semiconductor (H₂NC₄H₈NCH₂CH₂NH₂)(HNCH₂CH₂NH₂)₃Zn₂Ge₂Se₈ has been synthesized under solvothermal conditions using N-(2-aminoethyl)piperazine as solvent and templating agent at 200 °C. The material was characterized by single crystal and powder X-ray diffraction, IR and Raman spectroscopy and thermogravimetric analysis. The compound consists of 1D anionic [Zn₂Ge₂Se₈]⁴⁻ chains made of alternating edge-shared [ZnSe₄] and [GeSe₄] tetrahedra that charged balanced by one N-(2-aminoethyl)piperazinium and three piperazinium cations. The optical properties were investigated with solid state UV–Vis/near IR spectroscopy and the results show that the solid is a medium gap semiconductor with an absorption edge at 1.8 eV.     

NaBO2-NaCl-Na2CO3, NaBO2- Na2CO3-NaMoO4, NaBO2- Na2CO3-NaWO4, and NaBO2-NaCl-Na2WO4 ternary systems

The phase diagrams of the NaBO₂-NaCl-Na₂CO₃, NaBO₂-Na₂CO₃-Na₂MoO₄, NaBO₂- Na₂CO₃-Na₂WO₄, and NaBO₂-NaCl-Na₂WO₄ ternary systems were studied by a calculation-experimental method and differential thermal analysis. The coordinates of ternary eutectics were determined: E ₁: 612°C, 16 mol % NaBO₂, 42 mol % NaCl, and 42 mol % Na₂CO₃; E ₂: 568°C, 12 mol % NaBO₂, 28 mol % Na₂CO₃, and 60 mol % Na₂MoO₄; E ₃: 575°C, 12 mol % NaBO₂, 32 mol % Na₂CO₃, and 56 mol % Na₂WO₄; E ₄: 628°C, 8 mol % NaBO₂, 20 mol % NaCl, and 72 mol % Na₂WO₄; and E ₅: 655°C, 9 mol % NaBO₂, 53 mol % NaCl, and 38 mol % Na₂WO₄.     

Synthesis and characterization of inorganic solid electrolytes of Li2O-SiO2-P2O5 and Li2O-TiO2-SiO2-P2O5 systems

The lithium-ion-conducting inorganic solid electrolytes in the oxide systems Li₂O-SiO₂-P₂O₅ and Li₂O-TiO₂-SiO₂-P₂O₅ were prepared by the solid-state reaction, and the electrolyte pellet made by cold-pressing method had diameter of 13 mm and was about 1 mm thick. Phase identification and surface morphology of the products were carried out by X-ray diffraction and scanning electron microscopy. Ionic conductivity of the pellets was investigated through ac impedance. The results show that the adding of other cations can improve the ionic conductivity of the solid electrolyte, and the sintering temperature and duration can influence the ionic conductivity. The maximum ionic conductivity in the samples is 9.9 × 10⁻⁴ S/cm in the Li₂O-TiO₂-SiO₂-P₂O₅ system. Original Russian Text ? W. Li, M. Wang, Z.H. Li, X.F. Shang, H. Wang, Y.W. Wang, Y.B. Xu, 2007, published in Elektrokhimiya, 2007, Vol. 43, No. 11, pp. 1341–1345.     

Polymorphism in the Sc2Si2O7-Y2Si2O7 system

This paper examines the structural changes with temperature and composition in the Sc₂Si₂O₇-Y₂Si₂O₇ system; members of this system are expected to form in the intergranular region of Si₃N₄ and SiC structural ceramics when sintered with the aid of Y₂O₃ and Sc₂O₃ mixtures. A set of different compositions have been synthesized using the sol-gel method to obtain a xerogel, which has been calcined at temperatures between 1300 and 1750 °C during different times. The temperature-composition diagram of the system, obtained from powder XRD data, is dominated by the β-RE₂Si₂O₇ polymorph, with γ-RE₂Si₂O₇ and δ-RE₂Si₂O₇ showing very reduced stability fields. Isotherms at 1300 and 1600 °C have been analysed in detail to evaluate the solid solubility of the components. Although, the XRD data show a complete solid solubility of β-Sc₂Si₂O₇ in β-Y₂Si₂O₇ at 1300 °C, the ²⁹Si MAS-NMR spectra indicate a local structural change at x ca. 1.15 (Sc_2−xY_xSi₂O₇) related to the configuration of the Si tetrahedron, which does not affect the long-range order of the β-RE₂Si₂O₇ structure. Finally, it is interesting to note that, although Sc₂Si₂O₇ shows a unique stable polymorph (β), Sc³⁺ is able to replace Y³⁺ in γ-Y₂Si₂O₇ in the compositional range 1.86?x?2 (where x is Sc_2−xY_xSi₂O₇) as well as in δ-Y₂Si₂O₇ for compositions much closer to the pure Y₂Si₂O₇.     

Formation of [Cp2TiSbMe2]2, [Cp2TiSb(SiMe3)2]2 and [Cp2TiCl]2·2Mes4Sb2

Reactions of [Cp₂Ti(btmsa)] (btmsa = bis(trimethylsilyl)acetylene) with R₄Sb₂ (R = Me, Me₃Si) give [Cp₂TiSbMe₂]₂ (1) or [Cp₂TiSb(SiMe₃)₂]₂ (2) respectively. [Cp₂TiCl]₂·2Mes₄Sb₂ (3) is serendipitously formed from [Cp₂Ti(btmsa)] and Mes₂SbH containing NH₄Cl traces.