Synthesis of Thiourea Derivatives on Soluble Polymeric Support

A modified poly(ethylene glycol) (PEG) has been developed as the soluble polymeric supports for liquid phase synthesis of novel thiourea derivatives.In each step of the sequence,the PEG-bound products were precipitated in cold Et2O and the unreacted materials and by-products were removed by simple filtration.The progress of reaction,purity of the isolation and the structure of the PEG-bound products were easily monitored by TLC,IR and ^1H NMR spectra.Representative thiourea derivatives were obtained in moderate yields with excellent purity from this modified PEG-bound product by the cleavage with 50% TFA/H2O.     

Synthese und Kristallstrukturen der Phosphanimin-Komplexe MCl2(Me3SiNPMe3)2 mit M = Zn und Co,und CoCl2(HNPMe3)2

Syntheses and Crystal Structures of the Phosphaneimine Complexes MCl₂(Me₃SiNPMe₃)₂ with M = Zn and Co, and CoCl₂(HNPMe₃)₂ The molecular complexes MCl₂(Me₃SiNPMe₃)₂ (M = Zn, Co) have been prepared by the reaction of the dichlorides of zinc and cobalt with Me₃SiNPMe₃ in CH₃CN and CH₂Cl₂, respectively, whereas the complex CoCl₂(HNPMe₃)₂ has been prepared by the reaction of CoCl₂ with NaF in boiling acetonitrile in the presence of Me₃SiNPMe₃. All complexes were characterized by IR spectroscopy and by crystal structure determinations. The complexes MCl₂(Me₃SiNPMe₃)₂ crystallize isotypically. ZnCl₂(Me₃SiNPMe₃)₂: Space group P2₁2₁2₁, Z = 4, 2677 observed unique reflections, R = 0.024. Lattice dimensions at ?70°C: a = 1243.6; b = 1319.0; c = 1464.7 pm. CoCl₂(Me₃SiNPMe₃)₂: Space group P2₁2₁2₁, Z = 4, 3963 observed unique reflections, R = 0,071. Lattice dimensions at ?80°C: a = 1236.3; b = 1317.4; c = 1457.6 pm. CoCl₂(HNPMe₃)₂ · CH₂Cl₂: Space group Pbca, Z = 8, 1354 observed unique reflections, R = 0.055. Lattice dimensions at ?80°C: a = 1247.3; b = 998.4; c = 2882.4 pm. All complexes have monomeric molecular structures, in which the metal atoms are coordinated in a distorted tetrahedral fashion by the two chlorine atoms and by the nitrogen atoms of the phosphaneimine molecules.     

烟酸对酸性硫酸盐体系铜电沉积的影响

对溶液A: 0.8 mol•L－1硫酸铜,0.6 mol•L－1硫酸,5.0×10－5 mol•L－1氯离子,1.0×10－4 mol•L－1聚乙二醇的溶液,溶液B:在溶液A中加入2.0×10－2 mol•L－1烟酸,pH为0.5,运用循环伏安和计时安培法研究玻碳电极上铜的电沉积行为.结果表明,铜的电沉积过程经历了晶核形成过程,其电结晶按瞬时成核和三维生长方式进行.烟酸的加入对铜的电沉积具有阻化作用,但不改变铜的电结晶机理.沉积层的X射线衍射表明Cu为面心立方结构,在烟酸存在下沉积层出现(220)高择优取向,这可能是烟酸在Cu(220)晶面上发生强烈吸附作用的结果.     

粘度法研究高分子溶液行为的实验改进(Ⅱ)

高分子在粘度计毛细管管壁上的吸附不仅会导致毛细管有效管径减小，而且可以导致毛细管界面性质发生显著改变，具体表现为测定高分子溶液流过时间t之前和之后纯溶剂的流过时间t0和t0′与高分子溶液流过时间t对浓度作图外推到浓度为零时的值t0^*并不一致。不同温度时聚乙烯吡咯烷酮（PVP）水溶液粘度测定结果表明，当吸附讷发子显著改变了毛细管界面性质时，需要将高分子溶液粘度测定方法由t/t0′改为t/t0^*。经过改进的粘度测定方法不仅更加普适合理，而且更加简单有效。     

Preparation and characterization O-lauroyl chitosan/poly (L-lactic acid) blend membranes by solution-casting approach

O-Lauroyl chitosan/poly(L-lactide) (OCS/PLLA) blend membranes with different compositions were prepared by solution-casting approach using chloroform as common solvent. The experimental results of FT-IR, DSC and WAXD indicated that inter-association hydrogen-bond interactions existed between OCS and PLLA in the blend membranes. And SEM observation confirmed that the blend membranes with suitable compositions were compatible.     

Simultaneous Determination of Four Flavonoids in Pigeonpea [Cajanus cajan (L.) Millsp.] Leaves Using RP-LC-DAD

A simple and accurate RP-HPLC method using photodiode array detection (PAD) was developed for the simultaneous determination of four flavonoids, namely quercetin (QU),luteolin(LU),apigenin(AP) and isorhamnetin (IS) in pigeonpea leaves.Extract samples were separated on HIQ SIL C₁₈V column using methanol-acetonitrile-water(31:10:59, v/v/v) as mobile phase.The flavonoids were detected at 254.5 nm for QU and IS, and at 345 nm for LU and AP.Contents were determined with satisfactory repeatability (R. S. D. < 2.2%) and recovery (97.27 – 99.98%). The developed method was found to be simple and efficient.     

丽春红G-高碘酸钾催化光度法测定痕量锇

以Os(Ⅳ )催化高碘酸钾氧化丽春红G(PG)的褪色反应为基础 ,在 90℃加热 1 2min和 5 0 0nm波长处采用固定时间法测定丽春红G吸收值的降低 ,建立了测定痕量锇 (Ⅳ )的新方法。锇 (Ⅳ )的质量浓度在 0～ 0 48μg/L范围内呈良好的线性关系 ,检出限为 6 2× 1 0 - 9mg/L。对 0 4μg/L锇 (Ⅳ )测定的相对标准偏差为 0 71 % (n =1 1 )。催化反应对Os(Ⅳ )和丽春红G均为一级反应 ,催化反应的表观活化能为 78 80kJ/mol。所提出的方法在蒸馏分离后已应用于某些岩矿及冶金产品中锇的测定     

Cell detection based on protein array using modified glass slides

A protein array for cell detection was fabricated by spotting different antibodies on modified glass slides. Glass slides were modified to allow antibodies to be immobilized on it and to selectively bind antigens. Antibodies were specially selected with the cells to be detected as targets, which permitted target cells in samples to bind specifically to the array with little nonspecific binding. Results can be obtained by directly putting the samples onto the array for 1 h or a little longer to let the cells specifically interact with the antibodies. After washing the unbound samples away, images were observed with a microscope and captured with a CCD camera. The assessment of antibody-cell binding was evaluated by capturing red blood cells (RBCs) in human blood with blood group antibodies (anti-A and anti-B). Blood group antibodies were spotted on the modified glass slide and kept at 4<.deg> degrees C overnight for immobilization. Human blood samples diluted to different concentrations were used to examine the sensitivity and specificity of the method.     

Two Novel Sub-skeleton Types of ent-Kauranoids from Isodon gesneroides

Two novel ent-kauranoids with new sub-skeleton types, gesneroidins G and H were isolated as white powder from the ether extract of the leaves of Isodon gesneroides through normal phase column chromatography. Their structures were elucidated as 3β,6α,7β-triacetoxyl-15-hydroxyl-14-oxo-ent- 15,16-seco-kaur-11,17-olide and Iα-hydroxyl-3β,6α,7β,11 β-tetraacetoxyl-ent-nor-15,17-kaur-8,16-olide on the basis of the spectral evidences including ID and 2D NMR spectra.