新型Salen催化剂的合成及其在水解动力学拆分中的应用

文档编号:ZY048    文档字数:11266,页数:34

摘 要：手性环氧氯丙烷是一种极有价值的药物中间体，本文通过比较文献报道的几种方法，选取了水解动力学拆分法制备手性环氧氯丙烷。文中通过逐步嫁接的方法合成了壳聚糖固载的 (Salen)Co(Ⅲ)(OAc)催化剂，并建立了快速可靠的气相色谱法来跟踪检测产物(S)-环氧氯丙烷的对映体过量值（e.e.）。对反应条件进行单因素优化，发现反应在温度20℃，水用量为0.55当量，催化剂浓度为0.5mol%时，能够在10小时内得到对映体过量值>99%的(S)-环氧氯丙烷。
 
 关键词：手性环氧氯丙烷；水解动力学拆分；Salen催化剂 
 
 
Abstract: Chiral epichlorohydrin is a very important synton in organic synthesis. The hydrolytic kinetic resolution(HKR) of epichlorohydrin was chosed by compared with many methods reported. The Chitosan supported (Salen)Co(Ⅲ)(OAc) catalyst was synthesized via a stepwise and the enantiomeric excess of the (S)-epichlorohydrin was determined by GC analysis. Optimization of the conditions were investigated by the mono-factor’s experiment. Under the condition that the temperature was 20℃, the water was 0.55 equivalent, and the concentration of the catalyst was 0.5mol%, the enantiomeric excess (e.e.)of the (S)-epichlorohydrin was reach 99% within 10 hours .
 
Keywords：chiral epichlorohydrin; hydrolytic kinetic resolution(HKR);Salen catalyst
 
目  录
 中文摘要 I
 英文摘要 II
 目录 III
 1. 绪论 1
 1.1 引言 1
 1.2 研究现状  1
 1.3 文档研究内容 7
 2. 实验部分 8
 2.1 实验仪器与试剂 8
 2.2 催化剂合成 9
 2.3 水解动力学拆分环氧氯丙烷 14
3. 结果与讨论 15
 3.1 水解动力学拆分条件的优化  15
 3.2 催化剂的回收 18
 4．总结与展望 19
 4.1 总结 19
 4.2 展望 19
 致谢 20
 参考文献 21
 附录 23

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