论文 修改的4.docVIP

毕业设计(论文) 题 目 苯基咪唑并【5,6-f】 称 讲师 班 级 制药081班 学 号 20084570137 学生姓名 梁 盛 2012年6月1日 目 录 摘要 2 ABSTRACT 2 第一章 引言 4 1.1 前言 4 1.2 本课题提出的意义 5 第二章 实验部分 6 2.1仪器及试剂 6 2.2 1,10-邻菲罗啉5,6-二酮的合成的合成 摘要：1,10-邻菲罗啉在浓硫酸和溴化钾存在的条件下，用浓硝酸氧化得到1,10-邻菲罗啉5,6-二酮。将产物分离，测定其熔点，用1H-NMR和13C-NMR方法进行表征。通过跑板对反应进行了监控。实验过程中，设计不同的条件，分别就反应的温度、时间进行改变，得到合理的反应条件：反应开始时，滴加混酸时的温度控制在10℃之内，回流温度温度保持在100℃以上，回流时间选择在2小时。 将1,10-邻菲罗啉5,6-二酮与苯甲醛，醋酸铵和冰醋酸反应得到苯基咪唑并[5,6-f]邻菲罗啉。先将上述反应物反应得到淡黄色固体，然后用无水乙醇结晶即可得到苯基咪唑并[5,6-f]邻菲罗啉的晶体。测定熔点，并用1H-NMR等测试手段进行了表征。 1,10-邻菲罗啉；1,10-邻菲罗啉5,6-二酮；苯基咪唑并[5,6-f]邻菲罗啉；合成。3-pheny-l imidazo [ 5, 6-f ]- phenanthroline Abstract： 1,10-Phenanthroline was oxidated by concentrate nitric acid under the exist of concentrate sulfuric acid and potassium bromide, and yielded 1, 10-phenanthroline-5, 6-dione. The production was seperated and measured the melting point and characterized by 1H-NMR and 13C-NMR. During the reaction, TLC was used to monitor the reaction. We designed different conditions respectively on the changes of reacting temperature and reflux time. At last, a reasonable reaction conditions were sumerized: at the beginning of the reaction, the temperature of dropping mixed acid was controled below 10 ℃, reflux temperature was maintained at above 100 ° C, and the reflux time was chosen 2h. 1,10 - phenanthroline 5,6 - dione was reacted with benzaldehyde, ammonium acetate and acetic acid to yield phenyl-imidazo [5,6-f] phenanthroline. First of the reaction, the reactant above react to produce a yellow solid, and then use the anhydrous ethanol to crystallize the solid. A light yellow crystallization of phenyl-imidazo [5,6-f] phenanthroline then can be obtained. Determine the melting point of the crystallization, and characterized it by 1H-NMR and other testing means. Key words: 1,10-Phenanthroline monohydrate; 1 ,10-phenanthroline-5 ,6-dione; 3- pheny-l imidazo [ 5, 6-f