芳基-芳基偶联反应的研究进展

综述了近年来芳基-芳基偶联反应的研究进展, 包括不同类型芳基-芳基偶联反应的特点、机理和应用, 尤其是对立体选择性和区域选择性的偶联方法进行了重点介绍.     

具有双螺旋链的新型二维无机-有机骨架晶体材料Ni(PDC)(H2O)2的合成与结构

本文报道由H2PDC合成的新型维层状无机-有机骨架晶体Ni(PDC)(H2O)2(H2PDC=吡啶-2,5-二羧酸), 该化合物的一层是由右手螺旋Ni—O—C链与左手螺旋Ni-pdc链组成, 而邻近的一层则是由左手螺旋Ni—O—C链与右手螺旋Ni-pdc链组成, 层与层之间通过氢键作用形成了三维超分子结构. 用ICP、TG、IR和X射线单晶衍射分析等手段对其结构进行表征.     

某些新型冠醚-卟啉化合物的合成

本文以内消旋不对称单羟基-卟啉化合物1a～d合成了七种新型的冠醚-卟啉化合物3a～g和它们的中间体2a～g.这些化合物中的某些金属络合物对链烯的环氧化作用起催化作用, 它们的结构经元素分析,IR, UV和^1H NMR波谱证实.     

新型除草剂及其杂质的LC-MS和GC-MS分析

High performance liquid chromatography (HPLC) and electrospray ionization mass spectrometry (ESI-MS) have been utilized to analyze the synthesized 2-(2-arylaminomethylphenoxy)pyrimidine derivatives, which are a new kind of environmentally benign herbicides and have passed the temporary pesticide registration. The identification of main product and impurities has been achieved according to the UV and mass spectra. Moreover, one impurity, introduced by the raw material in the last step of the synthetic route, was identified by GC-MS analysis. It can be concluded that the combination of chromatography and mass spectrometry, including LC-MS and GC-MS, provided a vital tool of the pesticide science.     

茜素红与蛋白质分子Langmuir吸附聚集反应研究

在pH4.3的B-R缓冲体系中,用微相吸附-光谱修正技术[1]研究了茜素红(ARS)与牛血清白蛋白(BSA)、人血清白蛋白(HSA)的结合反应。其吸附结合常数分别为:KBSA-ARS=3.950×104,KHSA-ARS=4.377×104。染料与蛋白的最大结合数分别为NARS∶NBSA=9∶1,NARS∶NHSA=7∶1。经光谱修正技术计算结合产物的实际摩尔吸光系数分别为εBSA-ARS(537nm)=2.517×104L.mol-1.cm-1,εHSA-ARS(519nm)=2.051×104L.mol-1.cm-1,检出限BSA为19mg/L,HSA为23mg/L。经探讨该结合反应机理符合Langmuir吸附聚集反应方程。     

超分子钴(Ⅱ)配合物[CoL(H2O)2]n的合成与结构表征

A mononuclear Cobalt(Ⅱ) complex [CoL(H₂O)₂]_n (H₂L: 4,4′,6,6′-Tetrabromo-2,2′-[ethylenedioxybis(nitrilomethylidyne)]diphenol), has been synthesized and structurally characterized by elemental analysis, IR and X-ray diffraction single crystal structure analysis. The crystal of the complex belongs to monoclinic space group P2₁/c with a=2.516 8(3) nm, b=1.023 43(18) nm, c=0.789 17(14) nm, β=91.375(2)°, V=2.032 1(5) nm³, Z=4, D_c=2.317 Mg·m^-3, μ(Mo Kα)=8.747 mm^-1, F(000)=1 356, R₁=0.049 7, wR₂=0.110 4. The crystal structure of [CoL(H₂O)₂]_n indicates that the complex consists of one cobalt(Ⅱ) atom, one L^2- unit and two coordinated water molecules, and the coordination number of the cobalt(Ⅱ) atom is six. One-dimensional chain supramolecular structure is formed by intermolecular hydrogen bonds and π-π stacking of neighboring benzene rings. CCDC: 652649.     

异戊二烯稀土催化聚合过程中配合物结构及其转化的~(13)C-NMR研究

本文用~(13)C-NMR研究了异戊二烯(IP)在均相催化剂(CF_3CO_2)_2LnCl·EtOH—(i-Bu)AlH—o-C_6D_4Cl_2作用下的聚合过程。单体首先被活化同稀土配位生成η~4-IP稀土配合物(反式和顺式),然后η~4-IP的C-3和C-4插入Ln-H键生成η~3-烯丙基稀土配合物——η~3-(2-甲基)丁烯基稀土配合物(同式和对式)。二维~(13)C-NMR交换谱表明η~4-IP和0η~3-烯丙基的每对异构体在常温下分别进行慢交换反应(互变异构),这一过程使插入反应在常温下得以进行。     

Study on the Stereoselective Synthesis of Carbapenem Sidechain （2S,4S）-4-Acetylsulphanyl-2- [（S）-l-phenylethylcarbamoyl]- pyrrolidine-l-carboxylic Acid 4-Nitrobenzyl Ester

A stereoselective and economic synthesis of the carbapenem sidechain (2S, 4S)-4-ace-tylsulphanyl-2- [ (S) 1-phenylethyl-carbamoyl] pyrrolidine-l-carboxylic acid 4-nitrobenzyl ester was developed. Due to the effect of spatial hindrance, only the (2S,4S) diastereomer 3 was obtained by coupling 1 and the inexpensive racemic 2 catalyzed by EEDQ.     

Two new C18-norditerpenoid alkaloids from Aconitum delavayi

Further phytochemical investigation of the unique C18-norditerpenoid alkaloids from the roots of Aconitum delavayi Franch ledto the isolation of two new norditerpenoid alkaloids,delavaconitine F 1 and delavaconitine G 2.Their structures were determinedfrom spectroscopic evidence.     

Ion-ion reactions for charge reduction of biopolymer at atmospheric pressure ambient

Extractive electrospray ionization source(EESI)was adapted for ion-ion reaction,which was demonstrated by using a linear quadrupole ion trap mass spectrometer for the first ion-ion reaction of biopolymers in the atmospheric pressure ambient.