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 前言............................................................1 1.2 研究现状........................................................2 1.2.1以氢化钠作为催化剂.........................................2 1.2.2以金属钠作催化剂...........................................2 1.2.3以乙醇钠为催化剂...........................................2 1.3 实验设计........................................................4 2.实验部分.............................................................5 2.1 实验材料........................................................5 2.1.1 实验试剂..................................................5 2.1.2 实验仪器..................................................5 2.2 反应原理........................................................6 2.3 实验步骤........................................................6 2.3.1 缩合......................................................6 2.3.2 中和......................................................7 2.3.3 乙酰化....................................................7 2.3.4 分离纯化..................................................7 3.结果与讨论...........................................................8 3.1 对缩合过程中各因素的探讨........................................8 3.1.1不同催化剂对收率的影响.....................................8 3.1.2不同催化剂量对收率的影响...................................8 3.1.3不同溶剂对收率的影响.......................................9 3.1.4 不同反应时间对收率的影响..................................10 3.2 对中和过程中各因素的探讨........................................10 3.2.1不同酸对收率的影响........................................10 3.3 对乙酰化过程各因素的探讨........................................11 3.3.1 不同乙酰氯量对收率的影响..................................11 3.4 产物的表征......................................................12 4.总结与展望............................................................15 致谢....................................................................17 参考文献................................................................18 摘 要： 三氟乙酰乙酸乙酯是合成氟杂环医药和农药的中间体。本文阐述了以三氟乙酸乙酯和乙酸乙酯为原料，在碱性催化剂下进行Claisen缩合，并用质子酸进行中和，乙酰化等步骤合成三氟乙酰乙酸乙酯的方法。对合成三氟乙酰乙酸乙酯的反应条件进行了优化探讨，结果表明实验的最佳反应条件为：以环己烷为溶剂，1.2当量的金属钠为催化剂，反应物摩尔比为1：1.5，缩合反应时间为4小时，甲酸中和，以1当量的乙酰氯进行乙酰化，最后得到的收率为78%。 关键字：三氟乙酰乙酸乙酯；Claisen缩合; 乙酰化 Abstract: Ethyl-trifluoroacetoacetate is used as important intermediate in the synthesis of pharmaceutical or plant protection industry. This paper describe a way of preparation of ethyl-trifluoroacetoacetate by following steps . In the first step, ethyl-trifluoroacetate condensed with ethyl acetate in the presence of alkaline catalyst. The follow steps are neutralization and acetylation, then optimize the reaction conditions of the preparation of ethyl-trifluoroacetoacetate. The study show that the optimal reaction conditions as following: cyclohexane as solvent, 1.2 equivalent of sodium for catalyst, reactant molar ratio is 1 : 1.5, condensation reaction for 4 hours, formic acid for neutralization and 1 equivalent of chloride for acetylation, the yield of ethyl-trifluoroacetoacetate is 78%. Keywords: Ehyltrifluoroacetoacetate;；Claisen condensation；Acetylation