卟啉超分子化合物在分子器件中的应用

分子电子器件已成为近年来的一个研究热点，卟啉类化合物因为光敏性好、性能稳定、易于修饰等优点成为分子器件研究的理想模型化合物。本文着重介绍了它在分子器件中的最新应用进展。     

Synthesis of 3,5,7-Trioxapentacyclo[7.2.1.02,8.04,11.06,10]dodecane. A Novel Diacetal Trioxa-Cage

3,5,7-Trioxapentacyclo[7.2.1.0^2,8.0^4,11.0^6,10]dodecane, the parent compound of novel diacetal trioxa-cages, was synthesized from maleic anhydride cyclopentadiene adduct 1 by a four-step sequence. Attempts for the synthesis of monoaza dioxa-cage 12 failed. Ozonolysis of compound 9 in CH₂Cl₂-EtOH(1:1) at ?78°C followed by reduction with Me₂S gave 13 in 65% yield.     

氢化物发生石墨炉原位富集直接测定高温镍基合金中碲

通过选择碲的氢化物发生条件，克服了高含量镍对碲的干扰，把氢化物富集在涂钯石墨管里，然后再原子化，成功地测定了高温镍基合金中碲。     

Chemiluminescence flow system for the determination of ammonium ion

A novel chemiluminescence (CL) system for ammonium ion combined with flow-injection analysis is presented in this paper. It is based on the CL reaction between luminol, immobilized electrostatically on an anion-exchange column, and chlorine electrochemically generated on-line via a platinum electrode from hydrochloric acid in a coulometric cell. Ammonium ion reacts with chlorine and decreases the observed CL intensity. The system responds linearly to ammonium ion concentration in the range 1.0-100 muM, and the detection limit is 0.4 muM. A complete analysis, including sampling and washing, could be performed in 1 min with a relative standard deviation of <6.0%. The system is stable for over 500 determinations and has been applied successfully to the determination of ammonium ion in rainwater samples.     

人γ晶体蛋白的一级结构测定 1.γ晶体蛋白的分离提纯及其顺序测定方法(GC/MS法)的研究

成功地从人眼晶体中分离出单纯组分的γ晶体蛋白,对γ晶体蛋白的纯度、相对分子质量、氨基酸组成、N末端氨基酸组成等进行了测定,利用酸水解法和酶解法对γ晶体蛋白进行了水解和酶解条件的摸索、找出了使γ晶体蛋白断裂成适合于GC/MS联用仪进行结构测定的肽段的裂解条件。对进行氨基酸顺序测定的GC/MS法化学衍生化条件作了一系列的摸索,找出了化学衍生化的合适条件。对衍生化过程中的一些影响因素也进行了探讨。     

Polymer crystallization dynamics,as reflected by differential scanning calorimetry. Part 2: Numerical simulations

With the aid of a model for the kinetics of polymer crystallization, as put forward in previous publications, the shape of DSC-curves and their position on the temperature scale were simulated for various conditions of heat transfer in the apparatus. It turns out that the outcome is very dependent on the assumptions made with respect to these heat transfer conditions. For the ideal condition — no temperature differences between sample, pan and furnace — an invariable shape is predicted for the DSC-curves. They only shift to lower temperatures with increasing cooling rates. For more realistic conditions, the curves not only shift but become broader and their maxima decrease. They show a more familiar appearance. These calculations are very involved, however, A simple balance equation is shown to yield equivalent results, if a dimensionless characteristic number like the Nusselt number remains considerably smaller than one. This number contains an effective heat transfer coefficient between sample and furnace which, surprisingly, should not be too high. Apparently, the heat capacity of the pan does not play an important role under these conditions. This is investigated in Appendix II. Appendix I describes the procedure of the numerical simulations.     

Synthesis of N-methyl-3-aza[10] paracyclophane: A rigid analog of phenethylamine

The synthesis of N-methyl-3-aza[10]paracyclophane is reported which represents the first example of this ring system being formed via an acyloin reaction. This 3-aza[10]paraeyclophane ring system behaves physiochemically inbetween the normal [9]- and [10]paracyclophane ring systems. Reductive desulfurization of N-methyl-3-aza[10]paracyclophane-6-ethylene thioketal in ethanol provides a small amount of the title compound and an unexpected, ring-opened product, N-ethyl-N-methyl-p-heptylphenethylamine. A possible mechanism for the ring-opening process is suggested.     

人工神经元网络辅助丙烷氨氧化催化剂设计

报道了利用人工神经元网络辅助丙烷氨氧化制丙烯腈催化剂设计的研究进展结果．通过筛选得到了可以拟合该反应体系的神经元网络模型，从而使丙烷转化率和丙烯腈选择性可以表示为催化剂组成的函数，利用培训后的神经元网络模型所得到的权值文件，结合作者自编的优化程序，该网络可用于预测最优的催化剂组成．实验得到丙烯腈收率和选择性可分别达到４３．０％和５６．２４％．     

A Novel Approach to Synthesis of Tricyclic Diterpenoid

A novel approach has been found and the first total synthesis of (±)-Salvirecognine was accomplished by using it. In which intramolecular cyclization and Friedel-Crafts alkylation took place simultaneously to afford key intermediates for synthesis of aromatic tricyclic diterpenoids OMe PPA O O O OMe 1 2 Scheme 1 As shown in Scheme 1 intramolecular cyclization and Friedel-Crafts alkylation took place simultaneously when compound 1 was treated by PPA at 125 ℃. In which the i-pr…     

混合配体、希土三元配合物的研究 Ⅳ.3,5二硝基水扬酸(H2DNSA)、邻菲咯啉(phen)、希土(RE)三元固体配合物的合成及性质

本文报道了十种希土元素与3,5-二硝基水扬酸、邻菲咯啉三元配合物的制备方法。通过元素和化学分析测定了化合物的化学组成,并用红外光谱、紫外光谱、差热分析、磁化率、X射线粉天衍射等对所合成的化合物进行了结构和性质的研究。