苯乙酮与溴化铜合成α溴代苯乙酮的研究.docVIP

目 录 TOC \o 1-2 \h \z \u 摘要 Ⅰ-Ⅱ 1前言 1 2材料与仪器 4 2.1仪器 4 2.2试剂 4 3方法与结果 5 3.1反应方法 5 3.2产物定性 5 3.2.1薄层色谱定性（TLC法）定性 5 3.2.2熔点定性 6 3.2.3紫外分光光度法（UV）定性 7 3.2.4红外分光光度法（IR）定性 9 3.2.5定性小结 10 4产率优化 10 4.1反应温度对产率的影响 10 4.2溶剂对产率的影响 10 4.3原料投料比对产率的影响 11 4.4反应时间对产率的影响 12 4.5产率优化小结 13 5讨论 13 5.1反应方法与定性 13 5.2反应条件与优化 13 5.3问题与展望 14 参考文献 15 综 述 17 致 谢 22 PAGE PAGE 8 PAGE PAGE 7 苯乙酮与溴化铜合成α溴代苯乙酮的研究 中药学（中药分析鉴定方向） 摘要：目的 研究不同条件对苯乙酮与溴化铜合成α溴代苯乙酮的产率影响；方法 本实验通过使用苯乙酮和溴化铜反应制备α溴代苯乙酮，加热回流一定时间，趁热过滤，滤纸用溶剂冲洗，洗液与滤液合并，用水洗至中性，用分液漏斗分液取有机层，加无水硫酸镁干燥一段时间，过滤除去干燥剂，用旋蒸仪除去溶剂，冷却结晶得粗产品，粗产品经乙醇重结晶得白色针状晶体，通过控制不同的反应条件（溶剂、回流温度、投料比、回流时间）；结果 得到一定条件下苯乙酮与溴化铜合成α溴代苯乙酮的最佳合成条件；结论 苯乙酮与溴化铜的优化合成条件为：乙酸乙酯/氯仿（1：1）为溶剂，回流温度为62~63°C，苯乙酮与溴化铜投料比为1：2.2，回流时间为2个小时，产率最大 关键词：苯乙酮；溴化铜；α溴代苯乙酮；产率 Study on the synthesis of Acetophenone by acetophenone and copper bromide under different conditions Abstract: Objective Study on Synthesis and synthesis of alpha Acetophenone by different conditions. Method This experiment through the preparation of alpha bromoacetophenone using acetophenone and copper bromide reaction system, reflux time, hot filtering, filter paper using solvent cleaning lotion and the filtrate is washed with water to neutral, with a separatory funnel liquid from the organic layer, and absolute drying time of Magnesium Sulfate. Filtration to remove the desiccant, removing the solvent by a rotary steaming apparatus, cooling crystallization of crude products, crude product through recrystallization of white acicular crystal, by controlling different reaction conditions (solvent, reflux temperature, feed ratio, reflux time). Results Under certain conditions, the optimum conditions for the synthesis of Acetophenone with acetophenone and copper bromide were obtained. Conclusion The optimum conditions for the synthesis of Acetophenone and cupric bromide were as follows: ethyl acetate / chloroform (1:1) as solvent, refluxing temperature of 62~63 °C, the feed ratio of Ac