天然产物 6-脱氧-6氨基葡萄糖甘油糖脂的合成

天然氨基甘油糖脂sn-1,2-dipalmitoyl-3-(N-palmitoyl-6-dehydroxy-6-amino-α-glucosyl)glycerol 3 和 sn-1-palmitoyl-2-myristoyl-3-(N-stearoyl-6-dehydroxy-6-amino-α-glucosyl)glycerol 4 通过简便有效的合成策略首次被合成。其关键步骤为：三氯亚胺酯糖基供体 10 与 (S)-isopropyleneglycerol 在乙醚溶液中发生糖苷化反应,立体选择性的生成3-O-(2,3,4-tri-O-benzyl-6-dehydroxy-6-benzyloxycarbonylamino-α-D- glucopyranoyl)-1,2-O-isopropylene-sn- glycerol 7。中间体 7 经过脱除丙酮叉、与不同的脂肪酸缩合、脱除保护基和选择性的在氨基上酰化,最终得到目标化合物 3 和 4。     

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。     

Synthesis of 14-epi-19-nor-22-oxa-1α,25-dihydroxyvitamin D3

The synthesis of 14-epi-19-nor-22-oxa-1α,25(OH)2D3 5 was started from diol 8 via Fall's method, oxidation, epimerization, protection, coupling with the 19-nor-A-ring 7, and then deprotection of the hydroxyl functions.     

基于金属复分解闭环反应合成新型杯[4]冠醚衍生物

杯[4]芳烃的上端和下端通过金属复分解闭环反应以较高产率合成一系列新型杯[4]冠醚衍生物(8a-c),目标产物结构经元素分析、IR、MS、1H NMR及13C NMR证实。     

Thermal Decomposition and Dehydration Kinetics of Tetra(piperidinium) Octamolybdate Tetrahydrate in Air

Thermal decomposition of tetra(piperidinium) octamolybdate tetrahydrate, [C₅H₁₀NH₂]₄[Mo₈O₂₆]·4H₂O, was investigated in air by means of TG‐DTG/DTA, DSC, TG‐IR and SEM. TG‐DTG/DTA curves showed that the decomposition proceeded through three well‐defined steps with DTA peaks closely corresponding to mass loss obtained. Kinetics analysis of its dehydration step was performed under non‐isothermal conditions. The dehydration activation energy was calculated through Friedman and Flynn‐Wall‐Ozawa (FWO) methods, and the best‐fit dehydration kinetic model function was estimated through the multiple linear regression method. The activation energy for the dehydration step of [C₅H₁₀NH₂]₄[Mo₈O₂₆]·4H₂O was 139.7 kJ/mol. The solid particles became smaller accompanied by the thermal decomposition of the title compound.     

Differential and Integral Isoconversional Non‐linear Methods and Their Application to Energetic Materials. III. Non‐isothermal Decomposition Reaction Kinetics of Benzotrifuroxan

The thermal behaviour and decomposition reaction kinetics of benzotrifuroxan (BTF) were determined by TG and DSC techniques. The kinetic parameters of the exothermic decomposition reaction in a temperature programmed mode (the apparent activation energy Ea and pre-exponential factor A) were calculated by a single non-isothermal DSC curve. The E values calculated using the Kissinger and Flynn-Wall-Ozawa equations and integral isoconversional non-linear equations were used to check the validity of activation energy by a single non-isothermal DSC curve. The results show that the kinetic model function in integral form and the values of Ea and A of the decomposition reaction of BTFare , 109.95 kJ•mol－1 and 108.16 s－1, respectively. The values of ∆S≠, ∆H≠ and ∆G≠ of this reaction are －93.15 J•mol－1•K－1, 150.72 kJ•mol－1 and 153.15 kJ•mol－1, respectively. The critical temperature of thermal explosion of BTF is 257.33 ℃.     

微波辅助萃取-高效液相色谱法检测动物组织和牛奶中喹诺酮及非甾体类化合物

本文建立了一种快速的微薄辅助萃取-高效液相色谱法分离检测羊肝、牛肉和牛奶样品中三种喹诺酮类药物（氟罗沙星、洛美沙星和斯帕沙星）和两种非甾类化合物(酮洛芬和布洛芬)的方法。并对微波辅助萃取条件利用正交试验进行了优化：萃取温度为4℃、萃取时间为6min、萃取溶剂为乙腈、萃取溶剂体积为10mL。在浓度范围为0.25—0.75 μg•g－1时各待测物的三种不同水平的添加回收率在60.0%到107%之间,并获得较好的精确度（RSD＜11%）。     

Novel Strong Cation‐exchange Monolithic Column Using Poly(vinyl ester resin) as Stationary Phase Materials for Lysozyme Separation by HPLC

本实验合成了一种以聚乙烯基酯树脂为原料的聚合物整体柱。在聚合反应中,聚乙烯基酯树脂在聚合中既作为单体同时也作为交联剂,偶氮二异丁腈作为引发剂,十六醇为致孔剂。聚合物制得后以扫描电镜考察了该聚合物的内部形态。同时联合高效液相色谱分别考察了该整体柱的分离能力和载样量。在分离实验中,考察了流动相的浓度及pH值对分离效果的影响。结果表明,溶菌酶可成功的从鸡卵清中分离出,并在较短的时间内取得了较好的分离效果。     

Novel Zn（Ⅱ） ladder-like coordination polymer constructed from designed ferrocenyl ligand

Reaction of Zn（NO3）2·6H2O with 3-（4-carboxylphenylamino）-l-ferrocenyl-2-butylen-l-one （HL） and 4,4′-bipyfidine （4,4′- bipy） in methanol solution resulted in a novel ladder-like coordination polymer {[Zn2L2（μ2-L）2（4,4′-bipy）2]·MeOH}n （1）. Its crystal structure, thermal and electrochemical properties are presented.     

Synthesis and characterization of α-{ 3-[2-hydroxy-3- （N-methyl-N-hydroxy-ethylamino）propoxy]propyl}-ω- butylpolydimethylsiloxanes

α-{ 3-[2-hydroxy-3-（N-methyl-N-hydroxyethylamino）propoxy]propyl }-α-butylpolydimethylsiloxanes III with various molecu- lar weights were prepared by epoxy addition of α-[3-（2,3-epoxy-propoxy）propyl]-α-butylpolydimethylsiloxanes Ⅱ and N- methylmonoethanolamine. At each step, the outcome compounds were characterized through FT-IR and NMR spectra, the results showed that each step was successfully carried out and objective products were achieved.