Two salts of 5‐sulfosalicylic acid and 3‐aminopyridine

5‐Sulfosalicylic acid (5‐SSA) and 3‐aminopyridine (3‐APy) crystallize in the same solvent system, resulting in two kinds of 1:1 proton‐transfer organic adduct, namely 3‐aminopyridinium 3‐carboxy‐4‐hydroxybenzenesulfonate monohydrate, C₅H₇N₂⁺·C₇H₅O₆S⁻·H₂O or 3‐APy·5‐SSA·H₂O, (I), and the anhydrous adduct, C₅H₇N₂⁺·C₇H₅O₆S⁻ or 3‐APy·5‐SSA, (II). Both compounds have extensively hydrogen‐bonded three‐dimensional layered polymer structures, with interlayer homo‐ and heterogeneous π–π interactions in (I) and (II), respectively.     

哒嗪并[3,2-c]1,2,4-三唑类化合物的合成

以取代苯和丁二酸酐为起始原料, 经Friedel-Crafts反应, 肼合环, Br₂/HOAc氧化脱氢后得到一系列1,6-二氢-3-芳基-6-哒嗪酮(2a～2d). 然后将2a～2d与PCl₅在POCl₃中回流, 得到相应的氯代产物3a～3d, 将其与酰肼作用, 合环后得到一系列未见报道的哒嗪并[3,2-c]1,2,4-三唑类化合物. 所有化合物结构均经元素分析, IR, ¹H NMR 和MS谱得以证实, 并对其波谱性质进行了讨论.     

Fe（acac）3-Al（i-Bu）3-α，α＇-联吡啶催化丙烯腈与苯乙烯共聚合

研究了Fe（acac）3-Al（i-Bu）3-α，α＇-联吡啶（acac=乙酰丙酮）催化体系催化丙烯腈（AN）与苯乙烯共聚合，用元素分析和核磁共振研究了共聚物的结构，在单体比为1：1时共聚物中丙烯腈／苯乙烯含量分别为49．3％和50．7％．用凝胶渗透色谱研究了聚合物分子量和分子量分布，共聚物分子量分布较窄．动力学研究表明共聚合反应对单体浓度呈一级关系，表观活化能为57．8kJ／mol．     

Monoterpene Glycosides from the Roots of Paeonia lactiflora

The roots of Paeonia lactiflora Pall. is one of the most important traditional Chinese medicines, which has been used for the treatment of dizziness, spasm, menstrual disorder, spontaneous and night sweating, and as a general analgesic1. Chemical constitu…     

酚酞型聚芳醚砜(Ⅶ):K_2C0_3存在下PP/DCDPS体系聚合反应机理的研究

利用~(13)C-NMR方法研究了弱碱K_2CO_3存在下酚酞成盐反应及其与活性双卤砜亲核缩聚反应过程中的结构特征。对一系列碱性条件下酚酞(PP)与4,4'-二氯二苯砜(DCDPS)的缩聚反应的研究表明任何影响内酯结构酚酞盐生成的因素都会严重阻碍聚合反应的进行。对模型化合物存在下K_2CO_3在极性非质子溶剂中的溶解/解离行为的研究结果表明酚酞类Card。双酚与固体K_2CO_3之间可能存在着一种特殊的络合作用。基于我们系列研究结果,本文中总结提出了弱碱K_2CO_3存在下酚酞的反应机理。     

Maximum overlap symmetry molecular orbital model

This paper provides a brief and systematic presentation of the basic principle and method of the maximum overlap symmetry molecular orbital (MOSMO ) model and its application to simplification of molecular orbital calculation and to calculation of molecular structures and properties, together with some new results about the MOSMO calculation and new insights concerning the further extension of the principle and method. It has been shown that the theoretical method of the MOSMO model is very simple, reliable, and useful and can be employed to study the structure–property relation in even very large molecular systems. The numerical results obtained from the MOSMO calculation on various semiempirical molecular orbital approximation levels show that when the same parametrization, such as one of those employed in EHMO , CNDO /2, and HMO methods, is adopted, the MOSMOS are very close to the canonical molecular orbitals obtained from the customary LCAO method and the MOSMO calculation requires less computing time than does the LCAO method. The MOSMO calculation can be used for rapidly obtaining reasonably good molecular geometries, vibrational frequencies, and other properties of molecules by employing a simple improved semiempirical parametrization. Equilibrium geometries, vibrational frequencies, and other results are in good agreement with the experimental data and the results obtained from ab initio molecular orbital calculation. The basic calculational procedure of the MOSMO model can be extended further and has been employed to give some new results, to propose some new theoretical schemes and principles, and to introduce some new interesting theoretical problems that deserve to be studied further.     

十二烷基硫酸钠毛细管电泳法分析非还原单克隆抗体药物纯度的前处理条件优化

十二烷基硫酸钠毛细管电泳法因具有快速、分辨率高的优势，已成为单克隆抗体纯度分析的主流方法。在非还原单克隆抗体纯度检测中，其样品前处理过程对于结果有显著影响。为优化样品前处理，考察了以碘乙酰胺和N-乙基马来酰亚胺为巯基封闭剂，在pH 6.0~9.0的样品缓冲液条件下，不同种类和批次的单抗的纯度。发现在两种巯基封闭剂中，高pH的样品缓冲液会影响巯基封闭的效果，产生较多的抗体片段；而在低pH条件下，抗体片段较少，单抗的纯度更高。因此在进行非还原单抗的纯度检测中，pH 6.0的样品缓冲液为最佳的前处理条件。     

密闭微波辅助萃取当归粉中的阿魏酸

利用密闭微波样品制备系统(具有压力控制部件),对当归中的有效成分阿魏酸的萃取进行研究,比较了密闭微波萃取同超声波萃取和索氏萃取阿魏酸提取率的差异.结果表明:微波萃取与其他两种萃取方法相比,具有速度快和萃取率高的特点.并得到了阿魏酸提取的最佳条件:微波功率为400 W,萃取剂为90%的乙醇(体积分数),固-液比为1∶15,微波辐射为240 s,当归粒径为75μm.     

三苯甲基醚直接转化成丙酮化合物的反应

介绍了一种新的高效的由三苯甲基醚直接生成丙酮化合物的方法, 也就是使三氟乙酸条件下脱三苯甲基的反应和生成丙酮化合物的反应在一个反应瓶中同时进行, 使脱三苯甲基作用后生成的醇继续反应得到高产率的丙酮化合物. 这种方法对于分子中同时含有对酸敏感的其他官能团的三苯甲基醚分子的脱保护非常有用.