4,4′-(多苯基三联苯)双(有机硅烷)的合成

前文曾经报道利用四苯基环戊二烯酮为双烯体,乙烯基或烯丙基三乙氧基硅烷及其硅氧烷为亲双烯体通过Diels-Alder反应合成的多苯基芳基有机硅化合物作为硅橡胶的热     

Purification and partial characterization ofRhizomucor miehei lipase for ester synthesis

A commercialRhizomucor miehei lipase was purified by ammonium sulfate precipitation. Phenyl Sepharose 6 Fast Row hydrophobic interaction chromatography, and DEAE Sepharose Fast Flow anion-exchange chromatography. The recovery of lipase activity was 32% with a 42-fold purification. The molecular size of the purified enzyme was 31,600 Dalton and the pI 3.8. The enzyme was stable for at least 24 h within a pH range of 7.0-10.0, and 96.8% of the enzyme activity remained when kept at 30‡C for 24 h. Further, about 10–30% of the lipase activity was inhibited by K⁺, Li⁺, Ni⁺, Co²⁺, Zn²⁺, Mg²⁺, Sn²⁺, Cu²⁺, Ba²⁺, Ca²⁺, and Fe²⁺ ions and by SDS, but EDTA had no effect. Under the experimental conditions, the optimum temperature for the hydrolysis of olive oil was 50‡C (pH 8.0), and for the synthesis of 1-butyl oleate, 37‡C. It was concluded that hydrolytic activity of lipase alone is not a sufficient criterion for its synthetic potential. The optimal molar ratio of oleic acid and 1-butanol was 2:1 for 1-butyl oleate synthesis. The 1-butyl oleate yield was unaffected by purification of the enzyme after 12 h.     

Reaction of porous silicon with both end-functionalized organic compounds bearing alpha-bromo and omega-carboxy groups for immobilization of biomolecules

Both end-functionalized (alpha-bromo and omega-carboxy) compounds were first tested for the radical reaction on the silicon-hydride (Si-H) terminated porous silicon (PSi) with/without the presence of diacyl peroxide initiator under microwave irradiation. Then the carboxylic acid monolayers (CAMs) assembled on PSi through the robust Si-C bonds were converted to amino-reactive linker, N-hydroxysuccinimide (NHS)-ester, terminated monolayers. And finally two proteins of bovine serum albumin (BSA) and lysozyme (Lys) were immobilized through amide bonds. The optimum PSi membrane for protein immobilization without collapse, with parameters of porous radii 4-10 nm and depth 0.2-4.6 mum, was prepared from the (100)-oriented p-type silicon wafer. The chemically converted surface products were monitored with Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and field emission scanning electron microscopy (FESEM).     

过渡金属大环配合物的研究Ⅲ 4-硝基-苯并15冠-5与钴(Ⅱ)、铜(Ⅱ)和银(Ⅰ)配合物的合成及性质

有关冠醚配体与碱金属,碱土金属和稀土离子形成配合物的特性研究,国内外均有报导,但冠醚与d-过渡金属离子配合物的研究工作,则开展较晚,文献报导亦甚少。本文为探讨4-硝基-苯并15冠-5(No_2·B15C15)与过渡金属离子的配位能力,合成了Co(Ⅱ),Cu(Ⅱ),和Ag(Ⅰ)与4-硝基-苯并15冠-5配合物。并进行了元素分析,X-射线衍射,红外光谱,摩尔电导,激光拉曼光谱及差热-热失重分析的研究。     

新的聚合物支载硼氢负离子还原剂系统研究 3: 聚合物支载还原剂III

硼氢化钠的低分子还原系统研究很多,但其聚合物支载还原剂相对来说就很少,而且仅以强碱型阴离子交换树脂来制备的聚合物试剂。为了寻找用途更广泛的、新的聚合物支载还原剂,我们进行了硼氢负离子的聚合物还原系统的研究;发现能用弱酸型阳离子交换树脂制备出新的聚合物支载还原剂。前文报道了用NaBH_4的水溶液和阴离子交换树脂     

三核簇合物(Et4N)2[(CO)4MoS2MoS2Mo(CO)4]和(Et4N)2[(CO)4MoS2WS2Mo(CO)4]的合成及晶体结构

合成了含Mo(0)的三核化合物(Et₄N)₂[(CO)₄Mo(μ-S)₂Mo(μ-S)₂Mo(CO)₄](Ⅰ)和(Et₄N)₂[(CO)₄Mo(μ-S)₂W(μ-S)₂Mo(CO)₄](Ⅱ),测定了(Ⅰ)的晶体结构.Ⅰ属单斜晶系,空间群P2相似文献   

Sesquiterpenoids from the Rhizome of Ligularia virgaurea

Two novel sesquiterpene dimers, compounds 1 and 2 , were isolated from the rhizome of Ligularia virgaurea, together with the six known sesquiterpenoids 3 – 8 . Their structures were established by physico‐chemical and spectroscopic methods, especially by means of 1D‐ and 2D‐NMR as well as HR‐MS analyses. A mechanism based on a classical Diels–Alder cyclization is proposed for the formation of the dimer 1 from the precursors 8 and the quinone form of 6 (Scheme).     

一种新颖有机-无机杂化配位聚合物[(C10H16N)2（Pb2I6）·2DMF·H2O]n的自组装合成和晶体结构(英)

A novel coordination polymer [(C₁₀H₁₆N)₂（Pb₂I₆）·2DMF·H₂O]_n (C₁₀H₁₆N=N-butyl-2-Methy-Pyridinium) was synthesized by the reaction of Pb(NO₃)₂ with C₆H₁₀NI at room temperature in DMF solvent and structurally characterized by means of X-ray single diffraction. The title compound crystallizes in triclinic system, space group P1 with a=1.1237(2) nm, b=1.25330(16) nm, c=0.808 00(12) nm, α=102.523(4)°, β=92.475(5)°, γ=95.712(10)°, V=1.102 9(3) nm³, Z=1, D_c=2.470 Mg·m^-3, F(000)=738, chemical formula C₂₆H₄₈N₄O₃Pb₂I₆ and M_r=1 640.46, μ（MoKα）=11.849 mm^-1, the final R=0.057 8 and wR=0.166 5 for 3716 observed reflections with I > 2σ(I). The title compound consists of cations ([(C₁₀H₁₆N)⁺] and anion chain(PbI₃^-),they are combined by static attracting forces in the crystal. DMF and H₂O locate between the organic and inorganic moiety. CCDC: 210812.     

含噁二唑单元共轭聚合物合成与性质研究

单体 2 ,5 双 (4 溴苯 ) 1,3,4 二唑 (M Ⅰ )与 1,4 二乙烯基 2 ,5 二正丁氧基苯 (M Ⅱ ) ,在钯催化下通过Heck偶合反应合成得到共轭聚合物 ;单体和聚合物进行了1 H NMR ,1 3C NMR、质谱、FT IR、UV、荧光光谱、GPC、元素分析、热分析等测试 ;二唑 (OXD)基团是一种很好的生色团 ,对氧和热特别稳定 ,二唑环的亲电子性能使其特别适合于作为电子传输层 ,聚合物能发射很强的绿色荧光 ,它将是一类潜在的光电高分子材料     

手性5-l-(艹孟)氧基丁内酯并[3,4-d]-3-取代基-异(口恶)唑啉类化合物的合成

研究了手性元5-(R)-(l-(艹孟)氧基)-2(5H)-呋喃酮与取代苯甲醛肟以次氯酸钙作为氧化剂进行的区域选择性原位1,3-偶极环加成反应,同步生成两个新的手性中心,得到了一系列光学纯丁内酯并[3,4-d]-3-取代基-异(口恶)唑啉类化合物;应用波谱学手段及X射线单晶衍射法确证了产物的绝对构型,并对产物的核磁共振氢谱规律性加以总结.