Synthesis of Novel Bis(mesocyclic) polyamines

介绍了带羟基桥连双－（中环多胺）的合成。首先利用Ｎ－对甲苯磺酰基－３－羟基－１，５－二氮杂环庚烷与５种双官能基化合物在Ｎ２气氛下于无水乙腈中反应，得到５种带对甲苯磺酰基的中环多胺，然后利用ＨＢｒ／ＨＯＡｃ脱去保护基团，得到桥连双－（中环多胺）的氢溴酸盐。所有新化合物的结构均经ＩＲ、１ＨＮＭＲ、ＭＳ或元素分析证实。     

STUDY ON SYNTHESIS OF SELF CORSS LINKED POLYSTYRENE LATEX MICROSPHERES

Emulsifier-free emulsion polymerization of styrene in the presence of β-hydroxy propyl acrylate was studied.The emulsifier-free self cross linked polystyrene latex microspheres was obtained.Monomer conversion is higher than 90% when [St],[β-HPA],[KPS] is 2.66,0.228,and 5.8×10^-3mol/L respectively under 80℃ for 5h.The mono-dispersed latex particle diameter and colloidal particle concentration were given as D=0.23um,N=3.13×10^13/cm^3 by TEM analyse,The factors of influencing latex stability were discussed.Thecopolymer was characterized by IR and dissolution experiment.The apparent activation energy of polymerization and polymerization rate constant were obtained to be 78.7KJ/mol and 514.4/mol.s respectively.     

有机溶剂中(R)-醇腈酶催化不对称合成(R)-苯乙醇腈

 研究了来源于杏仁的（R）－醇腈酶在有机溶剂异丙醚中催化苯甲醛与HCN不对称合成（R）－苯乙醇腈，初步探讨了来源于不同杏仁的（R）－醇腈酶的筛选、最适酶量的确定以及底物HCN与苯甲醛的配比、底物浓度、酶的微环境pH和反应温度对不对称合成反应的影响．结果发现，来源于苦杏仁的（R）－醇腈酶优于来源于甜杏仁的（R）－醇腈酶．优化的反应条件为：最适酶量150g／L，HCN与苯甲醛的配比2．5，苯甲醛浓度300mmol／L，酶的微环境pH5．4，反应温度0～5℃．在该优化反应条件下，反应平衡转化率和产物的光学纯度均高达99％以上．     

化合物Cs5EuCl8·14H2O和Cs2EuCl5·4H2O的制备和荧光性

The two new compounds Cs₅EuCl₈·14H₅O(5∶1 type) and Cs₂EuCl₅·4H₂O(2∶1 type) were found and syn-thesized from CsCl-EuCl₃-11%HCl-H₂O quaternary systems by phase equilibrium method, and were characterized and measured by ultra-violet absorption spectrometry and fluorescence spectrum. The results show that upconversion spectrum exhibit at 590nm and 610nm exited at 790nm, and the upconversion intensity increases with the EuCl₃ ratio increasing in CsCl.     

血小板阻聚药物中间体N-环己基-5-氯丁基-1H-四氮唑的合成

以δ-戊内酯和环己胺为原料合成了抗血小板聚集药物西洛他唑的重要中间体N-环己基-5-氯丁基-1H-四氮唑，选择了合适的相转移催化剂及安全的叠氮试剂并获得较高的收率。     

二羟基丙酮磷酸酯的合成

本文报道由3-氯-1,2-丙二醇(1)经七步反应,合成二羟基丙酮磷酸酯缩乙酮(7)的方法,总收率43%。在温和条件下,7可以水解为游离的二羟基丙酮磷酸酯(8)。     

A Rapid Parallel Synthesis of 2-Dialkylamino-4（3H）-quinazolinones

2-Dialkylamino-4(3H)-quinazolinones 4 were rapidly synthesized by a solution-phase parallel synthetic method, which includes aza-Wittig reaction of iminophosphorane 1 with aromatic isocynate to give carbodiimide 2 and subsequent reaction of 2 with various aliphatic secondary amine in a parallel fashion.     

阿维菌素催化选择加氢合成伊维菌素研究

用RhCl3·3H2O和TPPDS间-(二磺化三苯基膦二钠盐),在水-有机两相催化体系中对阿维菌素选择加氢制备伊维菌素的研究,考察了反应温度(60～90℃)、氢气压力(1.0～4.0MPa)、配体浓度(2.2×10-3～5.2×10-3mol/L)、三乙胺浓度(0～8.4×10-4mol/L)、不同阳离子表面活性剂(TBAC:十四烷基二甲基苄基氯化铵;CPB:溴代十六烷基吡啶;CTAB:十六烷基三甲基溴化铵;TBAI:四丁基碘化铵)及反应时间对加氢反应活性和选择性的影响,其结果表明,在该两相体系中阿维菌素进行选择加氢是可行的,阳离子表面活性剂加入加快了反应速度,提高了反应的转化率和选择性.     

氯化原卟啉Ⅸ二甲酯合钴(Ⅲ)的合成及其与咪唑反应动力学的研究

从原卟啉Ⅸ（ＰＰⅨ）出发合成氯化原卟啉Ⅸ二甲酯合钴（Ⅲ），分别用元素分析，ＵＶ光谱和ＩＲ光谱表征。２９８Ｋ时，测定氯化原化原卟啉Ⅸ二甲酯合钴（Ⅲ）与咪唑反应在丙酮或二氯甲烷剂中的表观速率常数ｋｏｂ３，结果表明反应的决速步是单分子咪唑中间体Ｃｏ（Ⅲ）ＰＰⅨＤＭＥ（ＲＩｍ）Ｃｌ中氯的离解，总反应速率方程对咪唑是一级反应；氯离解的速率常数ｋ１依赖于溶剂与氯形成氢键的能力，即“远位咪唑氢键效应”；当咪唑中     

猪去氧胆酸化学 8:锇催化不对称双羟化合成 (24R,25R)-24,25,26-三羟基胆固醇

本文报道应用锇催化不对称双羟化对甾体化合物侧链三取代双键的反应合成得光学纯3a和3b,(3a∶3b=6.5:1),收率分别为71％和11％.从3a经五步反应合成新的维生素D_3类似物的关键中间体(24R,25R)-243 25,26-三羟基胆固醇(10).