3，7-二甲基-3-乙酰硫基-6-辛烯醛的水解反应研究
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