Three-component one-pot total syntheses of glyantrypine, fumiquinazoline F, and fiscalin B promoted by microwave irradiation

A microwave-promoted three-component one-pot reaction has been developed to provide access to the core pyrazino[2,1-b]quinazoline-3,6-dione (1) scaffold, which is common to several families of alkaloids with significant biological activities. By adapting this synthetic strategy through the use of selected Boc-amino acids and amino acid esters, we have accomplished highly efficient and concise total syntheses of glyantrypine (2), fumiquinazoline F (3), and fiscalin B (5), achieving overall yields of 55, 39, and 20%, respectively.     

铜(Ⅱ)-氨基酸水杨醛席夫碱-α-氨基酸三元配合物的稳定性研究

在25±0.1℃、I=0.1 mol·L^-1 KNO₃条件下，应用pH法测定了氨基酸水杨醛席夫碱(Sal∶A，A配体)-α-氨基酸(Aa,B配体)三元配合物的稳定常数，实验发现在三元配合物的稳定性与B配体的碱性之间存在良好的线性自由能关系。同时，以稳定性数据为探针，研究了三元配合物分子内存在的配体间疏水缔合作用。     

六(乙氧基吡咯烷酮)三聚磷腈的合成与表征

以N-羟乙基吡咯烷酮与氢化钠作用生成相应的钠盐,再将此钠盐与六氯三聚磷腈(HCCP)发生亲核取代反应,合成了六(乙氧基吡咯烷酮)三聚磷腈,用IR、31P NMR、1H NMR、13C NMR、DEPT、FABMS等现代谱学技术对其结构进行了表征。生物活性试验表明,此化合物1mg/mL时对腐生线虫Panagrellus redivivus的72h致死率为52·7%。     

氨基酸水杨醛席夫碱与铜(Ⅱ)配合物的合成及其抗菌活性和稳定性、结构间的关系

氨基酸水杨醛席夫碱与铜（Ⅱ）配合物的合成及其抗菌活性和稳定性、结构间的关系毕思玮＊刘树祥（曲阜师范大学化学系，曲阜２７３１６５）关键词：氨基酸水杨醛席夫碱铜（Ⅱ）稳定常数抗菌活性实验部分将１０ｍｍｏｌ氨基酸和０．５６ｇ（１０ｍｍｏｌ）ＫＯＨ溶于热的９...     

金属酞菁化合物在TiO2表面的分散研究

Dispersion of copper(Ⅱ) phthalocyanine (CuPc), copper(Ⅱ) phthalocyaninesulfonate (CuPcS) and cobalt(Ⅱ)phthalocyaninetetrasulfonate (CoPcTS) on the surface of titanium dioxide was investigated by XRD, XPS, FT-IR and UV-Vis techniques. Results show that interaction between CuPc and TiO2 was very weak and CuPc was difficult to disperse on the surface of the support. While partly sulfurized CuPcS could be dispersed on the surface of support through sulfo-groups and its dispersion capacity was determined to be 0.085 g CuPcS/g TiO2. Completely sulfurlzed CoPcTS could also be dispersed on the surface of TiO2 as a monolayer and its dispersion capacity was 0.12 g CoPcTS/g TiO2. Interactions of the sulfo-groups as well as the electrons of CoPcTS with the surface of TiO2 could be evidenced by FT-IR characterization. Therefore, it was suggested that CoPcTS molecules be adsorbed on the surface of TiO2 in a flat-lying mode while CuPcS in a slanting one. UV-Vis spectra show that the dispersed CuPcS and CoPcTS molecules exist in both forms of monomers and dimers.     

Analysis of fatty oil in Semen Ziziphi Spinosae by capillary gas chromatography

A simple and fast capillary gas chromatographic (CGC) method with flame ionization detection is developed for the analysis of fatty oil in Semen Ziziphi Spinosae. After methyl-esterification, eight components are identified by gas chromatography-mass spectrometry. The derivatization condition is investigated in order to validate this method. Palmitic acid and stearic acid are quantitated simultaneously. The limits of detection are 5.024 microg/mL for palmitic acid and 6.957 microg/mL for stearic acid, respectively. The limits of quantitation are 16.76 microg/mL for palmitic acid and 23.19 microg/mL for stearic acid, respectively. The percent recoveries of palmitic and stearic acid are 97.4% and 96.6%. CGC is shown to be a quick and informative tool for the analysis of fatty oil in Semen Ziziphi Spinosae.     

The synthesis and cationic polymerization of multifunctional silicon-containing epoxy monomers and oligomers

Several series of multifunctional silicon-containing epoxide monomers and oligomers have been prepared using rhodium catalyzed hydrosilation reactions. Dialkyl and diarylsilanes can be condensed with vinyl epoxides to give high yields of the desired diepoxides while the hydrosilation of alkyl and aryl silanes yields a mixture of di and tri epoxy substituted products. The condensation of αω,? Si? H difunctional compounds with vinyl epoxides can be carried out regioselectively to give α-hydrogen-ω-epoxy intermediates, which can be further reacted with di and tri olefins bearing terminal double bonds to give a series of well characterized epoxy functional oligomers. An investigation of the photoinitiated cationic polymerization of the monomers and oligomers, which were prepared during the course of these studies, was carried out. © 1994 John Wiley & Sons, Inc.     

Synthesis of triphenylamine-cored dendritic two-photon absorbing chromophores

[structure: see text]. A new series of dendritic two-photon absorbing chromophores containing triphenylamine moiety as a core or branching points have been synthesized through a convergent synthetic strategy. One-photon and two-photon optical properties of these molecules were characterized. In the nanosecond time domain, these molecules exhibited large two-photon absorption (TPA) cross sections up to 7.56-12.2 x 10(-44) s cm(4) at 800 nm, indicating that these molecular structures were viable candidates for various two-photon related applications.     

PHOTOSENSITIZATION SYSTEMS OF COVALENTLY LINKED PHTHALOCYANINE COMPLEXES IN BOTH BILAYER LIPID MEMBRANES AND TIN OXIDE PHOTOVOLTAIC CELL

Abstract Zinc phthalolocyanine photosensitized donor-acceptor systems for light energy conversion and for the design of photoelectrochemical molecular devices are presented. Covalently linked phthalocyanine complexes were incorporated in bilayer lipid membranes (BLM) and deposited on SnO₂ transparent electrodes. Their photovoltages were measured and compared. It has been found that a more favorable orientation and closer proximity are attained in the diad compounds between the donor (phthalocyanine)-acceptor (anthraquinone) pair than in the reference compound for efficient light-induced charge separation and transfer. The triad compound is the best among all tested compounds. The decrease in the fluorescence yield and lifetime induced by quinones was examined and the apparent electron-transfer rate constants were calculated.     

HPLC determination of ferulic acid in rat plasma after oral administration of Rhizoma Chuanxiong and its compound preparation

An HPLC method is described for determination of ferulic acid in rat plasma. The concentration of ferulic acid in rat plasma was determined after deproteinization with acetonitrile using sulfamethoxazole as internal standard. Chromatographic separations were performed on a C(18) stationary phase with a mobile phase composed of acetonitrile-water (16:84, v/v) with 1% glacial acetic acid. The UV detection wavelength was set at 320 nm. The method was successfully applied to the determination of pharmacokinetic parameters in rat plasma after oral administration of Rhizoma Chuanxiong and and its compound preparation Suanzaoren decoctions. The calibration curve was linear over the range 0.0510-4.08 micro g/mL in rat plasma. Within-day and between-day precisions were less than 4.5% RSD. Mean recovery was determined as 96.9%. The limit of quantitation was 0.0510 micro g/mL. The pharmacokinetic parameters of the two preparations were different significantly (p < 0.05), which may attribute to the effects of other ingredients present in Suanzaoren decoction.