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摘要：利用研磨的方法在无溶剂状态下进行苯乙酮的氯代反应，研磨法是利用研钵和研杵产生的机械力作用于反应物，而使反应进行的一种固相反应方法。它比传统的有机合成方法更方便和易于操作，在研磨条件下许多传统的反应可以在较温和的条件下进行，或者提高收率、或者缩短反应时间，甚至可以引起某些在传统条件下不能进行的反应。
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以苯乙酮，三氯异氰尿酸（TCCA），对甲苯磺酸为原料，利用研磨法在无溶剂条件下合成氯代苯乙酮，核磁共振光谱对产物进行分析，证明，研磨法不仅操作简单，而且对环境污染小。目前虽然存在很多氯代苯乙酮的合成方法，但是需要用到的试剂毒性很强，对人体和环境都会造成不同程度的危害。随着人们对生命科学和环境科学的深入了解，环保意识普遍得到提高，在此背景下，“绿色化学”的概念应运而生。如何减少有毒试剂的使用，减少有害废物的排放，就成为绿色合成化学的主要研究目标。在诸多的绿色合成方法中，机械研磨便是近年来发展起来的一种非常具有潜力的新颖的方法。20568
关键词：氯代苯乙酮；无溶剂；绿色化学，研磨法。
Rapid method for preparing chlorinated organics by grinding
Abstract: By using the method of grinding in solvent-free conditions for chlorinated reaction of acetophenone, grinding method is to use a mortar and pestle to produce mechanical force to the reactants, and make the reaction of a solid instead should method. It is more convenient than the traditional organic synthesis method and easy to operate, under the condition of the grinding of many traditional reaction can be under milder conditions, or to improve the yield and shorten the reaction time, and even can cause some reaction under the traditional condition.
With acetophenone,TCCA and p-toluene sulfonic acid as raw material,grinding under solvent-free conditions is for synthesis of chlorinated acetophenone.Nuclear magnetic resonance (NMR) spectroscopy and the analysis of the product proved that the grinding method is not only easy to operate,but also friendly-environmental.Although there are many methods for the preparation of chlorinated acetophenone, they need to use the highly toxic reagent and cause harm to human.With human's deeper understanding of the life science and environmental science, environmental protection consciousness is generally improved,and the concept of 'green chemistry' arises at the historic moment. How to reduce the use of poisonous reagent and the discharge of harmful waste, will become the main goal of green synthetic chemistry. In many green synthesis method, the mechanical polishing is developed as a very promising new method in recent years.
Key words : Chloroacetophenones; Solvent-free; Green Chemistry.
目 录
1 绪论 1
1.1研磨反应机理及影响因素 1
1.1.1 研磨反应机理 1
1.1.1.1 固态反应原理 1
1.1.1.2 研磨的作用 1
1.1.2 研磨反应的影响因素 1
1.1.2.1温度的影响 1
1.1.2.2催化剂的影响 1
1.1.2.3 原料的结构和配比影响 2
1.2研磨反应的应用 2
2 通过研磨法快速制备氯代苯乙酮的反应研究 6
2.1通过研磨法快速制备一氯代苯乙酮类化合物的反应条件优化 6
2.1.1 结果与讨论 6
2.1.2 实验部分 9
2.2通过研磨法快速制备一氯代苯乙酮类化合物的底物拓展 11
2.2.1 结果与讨论 12
2.2.2 实验部分 14
2.3通过研磨法快速制备二氯代苯乙酮类化合物的反应条件优化 15