摘要本论文的主要目标是研究如何利用柠檬醛和硫代乙酸来合成3,7-二甲基-3-乙酰巯基-6-辛烯醛，反应机理是一定比例的原料柠檬醛和硫代乙酸通过1,4-共轭加成反应合成3,7-二甲基-3-乙酰巯基-6-辛烯醛。最后再对粗产物进行分离提纯及结构鉴定。主要步骤：在室温条件下，先加入一定量的柠檬醛（2。5166g，97％，0。01653mol），再边搅拌边缓慢加入硫代乙酸（1。5078g，AR，0。01984mol），加入时间约为5-10分钟。加完后，控制油浴加热温度并保持温度至50℃，继续搅拌反应4。0小时，TLC分析跟踪反应至终点，得到3,7-二甲基-3-乙酰巯基-6-辛烯醛和原料的混合溶液。为得到纯度高的3,7-二甲基-3-乙酰巯基-6-辛烯醛，需要对混合溶液进行点板、提纯等一系列后处理操作。其中，用薄层层析的方法对产物进行提纯，柱层析我选择了V(乙酸乙酯)：V(石油醚) = 1:7展开剂用于本实验展开剂，将原料柠檬醛和产物3,7-二甲基-3-乙酰巯基-6-辛烯醛以及可能的副产物等进行分离。实验过程中持续使用点板对当前原料柠檬醛和产物3,7-二甲基-3-乙酰巯基-6-辛烯醛进行比对和确认，收集所需的目标产物。之后再进行相关的图谱分析。柱层析分离得到纯品后，分析纯品的三种图谱分析，可判断得到的产物是3,7-二甲基-3-乙酰巯基-6-辛烯醛。最后，通过设计合理的条件实验，得到最佳的合成3,7-二甲基-3-乙酰巯基-6-辛烯醛实验条件。71914

毕业论文关键词：柠檬醛；硫代乙酸；3,7-二甲基-3-乙酰巯基-6-辛烯醛；1,4-共轭加成反应；薄层层析；图谱分析。

Abstract The main objective of this paper is to study and analyze how to synthesize  3,7-dimethyl-3-acetylmercapto-6-octenal with citral and thioacetic acid , The reaction mechanism of the synthesis of 3,7-dimethyl-3-acetylmercapto-6-octenal is by the 1,4-conjugation addition of the raw material citral and thioacetic acid。 Finally, the crude product was separated and purified and its structure was identified。 The main steps: at room temperature conditions, first add a certain amount of citral（2。5166g，97％，0。01653mol）, and then slowly add thioglyphate（1。5078g，AR，0。01984mol） while stirring, adding time for about 5-10 minutes。 After the addition of the starting material, the temperature of the oil bath was controlled and maintained at a temperature of 50 ° C。 The reaction was continued for 4。0 hours。 TLC analysis followed the reaction to obtain a mixed solution of 3,7-dimethyl-3-acetylmercapto-6-octenal and a starting material。 In order to obtain a high-purity 3,7-dimethyl-3-acetylmercapto-6-octenaldehyde, it is necessary to perform a series of post-treatment operations such as dotting and purification of the mixed solution。 Among them, the product was purified by thin layer chromatography, and I chose V (ethyl acetate): V (petroleum ether) = 1: 7 as a developing agent for column chromatography, then the raw material citral and the product 3,7-dimethyl-3-acetylmercapto-6-octenal and the possible by-products are separated。 During the experiment continued use of point plate citral and 3,7-dimethyl-3-acetyl-mercapto-6-octenal for comparison and verification, the desired product was collected and combined desired。 The pure product obtained by column chromatography was analyzed by analyzing three different kinds of chromatograms, then the product was judged to be 3,7-dimethyl-3-acetylmercapto-6-octenal。 Finally, the optimum experimental conditions for the synthesis of 3,7-dimethyl-3-acetylmercapto-6-octenal were obtained by designing several reasonable control experiments。

Keywords::citral; thioacetic acid; 3,7-dimethyl-3-acetylmercapto-6-octenal; 1,4-conjugated addition reaction; thin layer chromatography;

目录

1。绪论 5

1。1背景