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硫代乙酸對檸檬醛的1,4-加成反應研究

時間:2019-06-14 20:49來源:畢業論文
通過硫代乙酸對檸檬醛的1,4-加成反應來制備硫酯以及通過柱分離得到3,7-二甲基-3-乙酰硫基-6-辛烯醛方法,最后再對其結構和可能產生的副產物進行分析研究

摘要:論文的主要目標是研究通過硫代乙酸對檸檬醛的1,4-加成反應來制備硫酯以及通過柱分離得到3,7-二甲基-3-乙酰硫基-6-辛烯醛方法,最后再對其結構和可能產生的副產物進行分析研究。用硫代乙酸與原料檸檬醛以1:1.2的比例在50℃條件下發生加成反應,得到3,7-二甲基-3-乙酰硫基-6-辛烯醛及可能的副產物的混合物產物5.16克,產率為77.7%。并對其進行萃取、干燥、柱層析等一系列后處理步驟后,得到較純的最終的目標產物,即3,7-二甲基-3-乙酰硫基-6-辛烯醛。其中,通過過柱子的方法對產物進行提純,用乙酸乙酯與石油醚的比例為1:20的溶液作為展開劑,將原料檸檬醛和產物3,7-二甲基-3-乙酰硫基-6-辛烯醛以及可能的副產物等進行分離后得到4.97克的產物,產率為77.7%。實驗過程中持續使用點板的方法對當前物料進行比對和確認,收集所需的目標產物并合并。之后再進行相關的圖譜分析,對最終產物進行核磁共振氫譜、紅外光譜和氣相色譜-質譜聯用的分析研究。36244
畢業論文關鍵詞:檸檬醛加成;硫代乙酸;3,7-二甲基-3-乙酰硫基-6-辛烯醛;柱層析
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.
源¥自%六:維;論-文'網=www.aftnzs.live

Key words: citral; Glucosinolates; thioacetic acid; 3, 7 - dimethyl - 3 - acetyl sulfonium - 6 - octene aldehyde; Column chromatography
目  錄
1 前言    1
1.1 背景    1
1.1.1 檸檬醛    2
1.1.2 硫醇類香料    2
1.1.3 縮硫醛酮類香料    2
1.1.4 硫醚類香料    2
1.1.5 硫酯類香料    3
1.1.6 硫代乙酸    3
1.2 文獻合成方法    2
1.2.1 硫代乙酸的合成    3
1.2.2 硫化氫加成反應    4
1.3 我的合成路線    6
2 試劑與儀器    8
2.1 試劑    8
2.2 儀器    9
2.3 裝置圖    9
2.3.1 還原反應裝置圖    10
2.3.2 旋轉蒸發儀裝置圖    10
2.3.3 柱層析裝置圖    11
3 實驗步驟    12
3.1 3,7-二甲基-3-乙酰硫基-6-辛烯醛的制備    12
3.2 產物的后處理    12 硫代乙酸對檸檬醛的1,4-加成反應研究:http://www.aftnzs.live/huaxue/20190614/34599.html
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