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含双催化中心手性氨基醇配体的合成及纯化_制药工程论文

发布时间:2015-04-02 来源:人大经济论坛
制药工程论文范文 目 录 中文摘要I 英文摘要II 目录III 1. 绪论1 1.1 研究手性药物的意义2 1.2 手性氨基醇及其应用3 1.3 手性氨基醇的合成4 1.4 手性氨基醇的发展前景5 2. 实验部分6 2.1 实验仪器6 2.2 实验试剂6 2.3 合成路线设计6 2.4 实验步骤7 2.4.3 色谱层析纯化8 2.5 本章小结8 2.6 流程图9 3. 结果与讨论10 3.1 实验结果10 3.2 实验讨论12 4.总结14 致谢15 参考文献16 摘 要:手性仲醇是天然产物及手性药物的重要合成砌块,也是合成具有手性功能材料的重要中间体,获得手性仲醇高对映体过量百分率(e.e.值)的重要方法之一是由手性氨基醇配体还原前手性酮获得。手性仲醇成为近年来最为活跃的研究领域之一。本论文在查阅相关资料的基础上综述了不对称催化还原反应研究新进展。 为了寻找性能优异的催化剂,基于多催化中心配体在不对称还原反应的协同效应,可获得手性仲醇较高的e.e.值。我们分别使用了(1S,2R)-(+)或(1R,2S)-(-)-2-氨基-1,2-二苯基乙醇为手性源与间二苄溴反应,经优化反应条件后在乙腈溶液中,于65℃下,以KI为催化剂,K2CO3为吸氢剂首次合成了含双催化中心配体,N-(1'R,2'S)-(1',2'-二苯基-2'-羟基) 乙基-间二苄胺和N-(1'S,2'R)-(1',2'-二苯基-2'-羟基)乙基-间二苄胺,经过硅胶柱色谱纯化得无色晶体,获得较好的产率。 关键词:手性氨基醇;配体;合成;纯化 Abstract: Chiral alcohols is a natural product and the importance intermediate of chiral drugs synthesis as well as chiral synthesis of functional materials. One of the important ways to acquire chiral secondary alcohols high enantiomeric excess percentage(e.e.value) is by chiral amino alcohols ligand catalytic reduction of prochiral ketone access. Chiral alcohol has become one of the most active research areas in recent years. In this paper, the inspection on the basis of relevant information summarizes the asymmetric catalytic reduction reaction of new progress. In order to find high performance catalyst remains, based on more catalysis center ligand in asymmetric catalytic reduction of synergies, can achieve available chiral secondary alcohols higher e.e.value. We were respectively using (1S,2R)-(+) and (1R,2S)-(-)-2-amino-1,2-diphenyl ethanol as chiral sources with 1,3-benzyl bromide reponse by optimizing the reaction conditions in acetonitrile solution, in 65℃, KI as a catalyst and K2CO3 as a hydrogen absorption reagent first synthesized the catalysis center with two ligand, N-(1'R,2'S)-(1',2-diphenyl-2'-hydroxyl) ethyl-1,3-benzyl amine and N-(1'S,2'R)-(1',2-diphenyl-2'-hydroxyl) ethyl-1,3-benzyl amine, by silica gel column chromatography get the colorless crystal. It has good yield. Keywords:Chiral Amino Alcohols;Ligand ; Synthesize ; Purify
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