论文编号:ZY048论文字数: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 论文研究内容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
新型Salen催化剂的合成及其在水解动力学拆分中的应用......