摘要：论文的主要目标是研究通过水解3，7-二甲基-3-乙酰硫基-6-辛烯醛的方法制备3，7-二甲基-3-巯基-6-辛烯醛的反应以及通过柱分离试验验证是否可以得到3，7-二甲基-3-巯基-6-辛烯醛的方法，最后再对其结构和可能产生的副产物进行分析研究。氢氧化钠的水溶液与原料3，7-二甲基-3-乙酰硫基-6-辛烯醛发生水解反应，得到3，7-二甲基-3-巯基-6-辛烯醛及可能的副产物的混合物产物，并对其进行萃取、干燥、旋转蒸发、柱层析等一系列后处理步骤后，由于产物和原料极性相近，无法完全分离，得到的是产物和原料的混合物。其中，乙酸乙酯与石油醚的比例为1:10的溶液作为展开剂。实验期间中持续使用点板的方法对当前溶液进行比对和确认，收集所需的目标产物并合并。之后再进行相关的图谱分析，对最终产物进行液相色谱-质谱联用的分析研究。根据LC-MS图谱，理论产率到达93.4%。27823
毕业论文关键词：乙酰硫基，水解反应，巯基，薄层析,液相色谱-质谱联用
Research on hydrolysis reaction about 3,7-dimethyl
-3-mercapto-6-octenal
Abstract:This paper mainly aims to study the conditions for 3,7-dimethyl-3-sulfydry
-6-octenal preparation through hydrolysis reaction of3,7 -dimethyl-3-mercapto-6-
octenal as well as testing the preparation method through column separation..Finally, the paper studied the structure of by-products that may be produced.The hydrolysis reaction between aqueous solution of sodium hydroxide and raw material 3,7-dimethyl-3-sulfydryl-6-octenal can produce the mixture of 3,7 -dimethyl-3-sulfy
-dryl-6-octenal and possible by-products.A series of post-processing on the mixture,such as extraction, drying, rotary evaporation,column chromatography,etc.,
unenable to get the final pure target products: 3,7-dimethyl -3-sulfydryl-6-octenal.Be
-cause the polarity of the product and the raw is so close that we cannot separate them completely.Next the raw,product and possible by-products were separated by developing solvent of ethyl acetate and petroleum ether (1:10).During the experiment, materials were compared and confirmed through continuous point plate, thus enabling to collect desired target products and integrating them. Next, the final product was analyzed through liquid chromatography-mass spectrometry (LC-MS). According to LC-MS, the theoretical yield is 93.4%.
Key words:mercapto,hydrolysis reaction,sulfydryl,thin layer chromatography,LC-MS
目 录
1 前言 1
1.1香精香料简介 1
1.1.1按香来源分类 1
1.1.2按剂型分类 1
1.1.3按用途分类 1
1.1.4按香型分类 1
1.2香精香料安全问题 2
2 文献合成方法 3
2.1含硫香料 3
2.2水解反应 4
2.3典型类型 4
2.3.1卤化物的水解 4
2.3.2酯的水解 4
2.3.3胺的水解 5
2.3.4硫酯基的水解 5
2.4硫醇类香料的一般合成方法 6
2.4.1醇与硫化氢反应 6
2.4.2卤代物与硫化氢反应 6
2.4.3卤代烷与硫氰化钾或硫氢化钠反应 6
2.4.4卤代烷和硫脲反应 6
2.4.5卤代烷与硫代硫酸盐反应 7
2.4.6烯烃与硫化氢加成 7
2.5文献合成方法 7
2.5.1光学活性3-巯基己醇及乙酸酯的合成路线 7
2.5.2异丙硫醇的合成 8
2.5.3正丁硫醇的合成 9
2.5.4二苄基二硫醇的合成 9 3，7-二甲基-3-乙酰硫基-6-辛烯醛的水解反应研究:http://www.youerw.com/huaxue/lunwen_22466.html