摘要：论文的主要目标是研究通过硫代乙酸对柠檬醛的1,4-加成反应来制备硫酯以及通过柱分离得到3,7-二甲基-3-乙酰硫基-6-辛烯醛方法，最后再对其结构和可能产生的副产物进行分析研究。用硫代乙酸与原料柠檬醛以1:1.2的比例在50℃条件下发生加成反应，得到3,7-二甲基-3-乙酰硫基-6-辛烯醛及可能的副产物的混合物产物5.16克,产率为77.7%。并对其进行萃取、干燥、柱层析等一系列后处理步骤后，得到较纯的最终的目标产物，即3,7-二甲基-3-乙酰硫基-6-辛烯醛。其中，通过过柱子的方法对产物进行提纯，用乙酸乙酯与石油醚的比例为1:20的溶液作为展开剂，将原料柠檬醛和产物3,7-二甲基-3-乙酰硫基-6-辛烯醛以及可能的副产物等进行分离后得到4.97克的产物,产率为77.7%。实验过程中持续使用点板的方法对当前物料进行比对和确认，收集所需的目标产物并合并。之后再进行相关的图谱分析，对最终产物进行核磁共振氢谱、红外光谱和气相色谱-质谱联用的分析研究。36244
毕业论文关键词：柠檬醛加成；硫代乙酸；3,7-二甲基-3-乙酰硫基-6-辛烯醛；柱层析
The 1, 4 - addition reaction of  thioacetic acid and citral
Abstract: This paper mainly aims to study The 1, 4 - addition reaction of thioacetic acid and citral to preparation of 3, 7 - dimethyl - 3 - acetyl sulfonium - 6 - octene aldehyde method, they react with proportion of 1:1.2 amount of substance.,and produce 5.16g 3, 7 - dimethyl - 3 - acetyl sulfonium - 6 - octene aldehyde,and the productive rate is 80.6% .Finally, the paper studied the structure and may produce by-products. Generation of thioacetic acid with sulfur addition reaction with raw material citral, get 3, 7 - dimethyl - 3 - acetyl sulfonium - 6 - octene aldehyde and may be a mixture of the by-products of product, and carries on the extraction, drying, column chromatography and a series of processing steps, get a pure product of the final goal is 3, 7 - dimethyl - 3 - acetyl sulfonium - 6 - octene aldehyde. Among them, the purification of product by using the method of a pillar, with the ratio of ethyl acetate and petroleum ether solution as an agent for 1:20, and we got 4.97g 3, 7 - dimethyl - 3 - acetyl sulfonium - 6 - octene aldehyde .The productive rate is 77.7%.citral and product materials will be in 3, 7 - dimethyl - 3 - acetyl harvard - 6 - octene aldehyde and possible by-products such as separation. Last point plate in the process of experiment method to compare the current material and confirmation, collect the target product and merge. Before the relevant map analysis, the final product for nuclear magnetic resonance hydrogen spectrum, infrared spectrum and gas chromatography - mass spectrometry analysis.
Key words: citral; Glucosinolates; thioacetic acid; 3, 7 - dimethyl - 3 - acetyl sulfonium - 6 - octene aldehyde; Column chromatography
目  录
1 前言    1
1.1 背景    1
1.1.1 柠檬醛    2
1.1.2 硫醇类香料    2
1.1.3 缩硫醛酮类香料    2
1.1.4 硫醚类香料    2
1.1.5 硫酯类香料    3
1.1.6 硫代乙酸    3
1.2 文献合成方法    2
1.2.1 硫代乙酸的合成    3
1.2.2 硫化氢加成反应    4
1.3 我的合成路线    6
2 试剂与仪器    8
2.1 试剂    8
2.2 仪器    9
2.3 装置图    9
2.3.1 还原反应装置图    10
2.3.2 旋转蒸发仪装置图    10
2.3.3 柱层析装置图    11
3 实验步骤    12
3.1 3,7-二甲基-3-乙酰硫基-6-辛烯醛的制备    12
3.2 产物的后处理    12 硫代乙酸对柠檬醛的1,4-加成反应研究:http://www.751com.cn/huaxue/lunwen_34599.html