新型主体试剂交联聚合β-环糊精-邻香草醛苯甲酰腙的合成及荧光法识别锌

合成了新型主体试剂交联聚合 β 环糊精 邻香草醛苯甲酰腙 (β CDP OVBH) ,探讨了与Zn2 + 的荧光识别反应。在pH =8.30的NH3·H2 O NH4 Ac ,5 .0 0mLDMF中 ,β CDP OVBH与Zn2 + 络合生成 1∶1的包合物 ;线性范围 2 .5 0～ 5 0 0 μg L ;检测限 0 .6 0 8μg L ;2 8种常见离子干扰实验的研究 ,显示出该主体试剂对客体Zn2 + 有较高的选择识别效果。方法简便、快速地用于茶叶、人发中痕量锌的测定 ,结果满意。     

水杨醛-1H-苯并三唑乙酰腙与RE(III)配合物的热化学

在甲醇中,合成了6种稀土与水杨醛-1H-苯并三唑乙酰腙(C15H13N5O2,简称SBTH)的新配合物RE(HL)2ClO4(RE=Pr, Nd, Sm, Eu, Gd, Tb; HL=C15H12N5O2),并对其进行了元素分析、摩尔电导率、IR和1H NMR的测定,确定了其组成.通过TG-DTG、DSC研究了配合物的热分解过程,得到了各配合物的分解焓,利用Kissinger法及Ozawa法计算出各配合物主要分解阶段的表观活化能,测量了该系列配合物在二甲基甲酰胺(DMF)中不同浓度时的溶解焓.     

吲唑类化合物合成新方法的研究（Ⅰ）

本文研究了2,6-二烷氧基苯乙酮腙在多聚磷酸(PPA)存在下受热脱去一分子醇环化生成3-甲基-4-烷氧基吲唑的合成反应.并研究了水杨醛、邻甲氧基苯甲醛、2,4-二羟基苯甲醛以及邻羟基苯乙酮、2-羟基-3,5-二甲基苯乙酮腙在PPA存在下的受热反应过程.     

微波促进的5-氯-3-甲基-1-苯基-4-吡唑甲醛与氯化N-苯乙酮基吡啶及芳酰肼的缩合反应

5-氯-3-甲基-1-苯基-4-吡唑甲醛(1)在微波辐射下, 与氯化N-苯乙酮基吡啶(2)和取代苯乙酮3在醋酸铵/醋酸体系中一锅煮反应, 高产率地生成了吡唑基取代的吡啶衍生物4a～4e. 1与芳酰肼在微波辐射下反应, 则形成了酰腙类化合物6a～6g. 1与羟胺在微波辐射下缩合可生成肟7a和腈7b的混合物.     

Syntheses,Structures and Characterizations of Two Vanadium(V) Complexes:[2-MePyH][V^vO2(C14H9N2O3Br)] and [2-EtPyH][V^VO2(C14H9N2O3Br)]

Two new oxovanadium(V) complexes, [2‐MePyH][V^vO₂(L)] (3) and[2‐EtPyH][V^vO₂,(L)] (4) (salicylaldehyde 5‐bromo salicyloylhydrazone is abbreviated as H₂L; 2‐MePyH is protonated 2‐Mepyridine; 2‐EtPyH presents protonated 2‐Et‐pyridine) were obtained from a reaction of VOSO₄ and H₂L in acetonitrile‐methanol with small quantity of 2‐Me‐pyridine or 2‐Et‐pyridine, and characterized by X‐ray diffraction and spectroscopic methods. Crystal data: [2‐MePyH][VO₂(L)] (3), C₂₀H₁₇N₃O₅BrV, M_r = 510.2, monoclinic, P2₁/n, a = 0.7363(1) nm, 6 = 0.9514(1) nm, c = 2.8594(2) nm, β = 95.305(2)°, Z = 4 and V=1.9946(3) nm³, μ(Mo Kα) = 2.539 mm^?1; [2‐EtPyH][VO₂(L)] (4), C₂₁H₁₉N₃ O₃BrV, M_r = 524.2, triclinic, P1 , a = 0.8051(1) nm, b = 0.9413(1) nm, c = 1.4648(2) nm, α=99.1900(10)°, α = 99.4530(10)°, γ = 104.6670(10)°, Z = 2 and V= 1.0355(2) nm³, μ(Mo Kα) = 2.448 mm^?1, X‐Ray analyses revealed that the crystal structures of 3 and 4 have similar packing modes.     

二苯卡巴腙键合硅胶固定相的制备及对重金属离子的选择性分离富集研究

制备了二苯卡巴腙键合硅胶,研究了此键合硅胶的性质及对常见重金属离子的分离富集行为,发现对水中痕量Hg(Ⅱ)有好的选择性富集效果,通过实验对富集条件进行了选择。研究结果表明:对Hg(Ⅱ)的最大富集率可达100%,最大吸附量为1.84×10-3mmol g。该键合硅胶对于水中痕量Hg(Ⅱ)的富集分离与测定具有较高的灵敏度和较好的富集作用,富集倍率为540。可在Cd(Ⅱ)、Ni(Ⅱ)、Co(Ⅱ)、Mn(Ⅱ)等多种金属离子存在下对Hg(Ⅱ)进行选择性富集。     

Synthesis and Crystal Structure of a Vanadium（V） Complex with 2-Hydroxy-1-naphthaldehyde Isonicotinoyl Hydrazone

The mononuclear vanadium(Ⅴ) complex with 2-hydroxyl-1-naphthaldehyde isoncotinoyl hydrazone was synthesized and characterized by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P2 1/n with a = 10.3153(15),b = 7.4024(11 ),c = 24.413(4) (A),β= 101.911(2)°,V= 1824.0(5) (A)3,Z = 4,Mr = 427.28,Dc = 1.556 g/cm3,F(000) = 880,μ(MoKα) =0.591,the final R = 0.0372 and wR = 0.0926.The vanadium(Ⅴ) atom adopts a distorted square-pyramidal geometry coordinated by the tridentate ligand and two oxygen atoms.The hydrogen bonds and strong π…π stacking interactions link the complex molecules into a 3-D network structure.     

配合物Cu(C14H10N2O2)(C5H5N)的合成和晶体结构

The novel copper(Ⅱ) complex with salicylaldehyde benzoylhydrazone and pyridine ligands， Cu(C₁₄H₁₀N₂O₂)(C₅H₅N)， has been synthesized and characterized by elemental analysis， IR and thermal analysis. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group P2₁/c. The cell parameters are： a=1.6362(9)nm， b=1.7140(9)nm， c=1.2255(7)nm， β=105.168(9)°， V=3.317(3)nm³， Z=8， D_c=1.525g·cm^-3， μ(MoKα)=1.334mm^-1， F(000)=1560. The structure was refined to final R₁=0.0376， wR₂=0.0909. The copper(Ⅱ) ion lies in a dis-torted square-planar environment composed of two oxygen atoms， one nitrogen atom of tridentate acyhydrazone Schiff base ligand and one nitrogen atom of the pyridine ligand. CCDC： 193111.     

3,5-二苄氧基苯甲酰水杨醛腙的合成及其与稀土硝酸盐配位性能的研究

合成了配体3,5-二苄氧基苯甲酰水杨醛腙(HL)及其与稀土硝酸盐的五种配合物. 通过元素分析、红外光谱、紫外光谱、摩尔电导等测试手段确定配合物组成为[Ln2(L)3(NO3)2](NO3) (Ln = Sm3+, Eu3+, Gd3+, Tb3+, Dy3+), 并对其进行了表征.     

对苯双酰腙类化合物的合成与表征

以对苯二甲酸为起始原料,设计合成了5个新型的对苯双酰腙类化合物,其结构经1H NMR,MS和元素分析表征。