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摘要：论文的主要目标是研究通过环氧柠檬醛在稀硫酸-乙腈系统中重排，生成2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛，并找出合适的方法将它提纯分离。6、7-环氧柠檬醛与在酸性条件下的乙腈会发生缩合反应，生成2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛及其异构体，并进行萃取、干燥、旋转蒸发、柱层析等处理后，得到较纯的最终的目标产物，即2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛。通过硅胶柱层析的方法对产物进行提纯，用乙酸乙酯与石油醚的比例为1:2的溶液作为展开剂，将原料柠檬醛、产物以及可能的副产物等进行分离。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。同时对收集的组分进行图谱分析，对所得到的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。根据实验结果，产率达到45%左右。36246
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毕业论文关键词：环氧柠檬醛；重排反应；2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛；柱层析
2- (5- (2-hydroxy-2-yl) -2-methyl-tetrahydrofuran-2-yl)
acetaldehyde Separation and purification
Abstract:The objective of this paper is to study the epoxy citral in sulfuric acid - acetonitrile system rearrangement to form 2- (5- (2-hydroxy-2-yl)-2-methyl-tetrahydrofuran-2-yl) acetaldehyde and identify suitable methods to get it. 6,7-epoxy-citral acetonitrile under acidic conditions, the condensation reaction will occur to form 2- (5- (2-hydroxy-2-yl) -2-methyl-tetrahydrofuran-2-yl) acetaldehyde and its isomer , and extracted, dried, rotary evaporation, column chromatography treatment, to give relatively pure final target product, i.e., 2- (5- (2-hydroxy-2-yl) -2-methyl-tetrahydrofuran-2-yl) acetaldehyde. By way of silica gel column chromatography product was purified using the ratio of ethyl acetate and petroleum ether 1: 8 as developing solvent solution, the separated material citral, products and by-products, etc. may be. During the experiment continued use point plate method to compare the current material and identify, collect and merge the desired target product. While the components collected profiling of the product was subjected to nuclear magnetic resonance spectroscopy, infrared spectroscopy and gas chromatography - mass spectrometry analysis. According to the results, the yield of about 50%.
Keywords: epoxy citral; rearrangement reaction;column chromatography;
2- (5- (2-hydroxy-2-yl) -2-methyl-tetrahydrofuran-2-yl) acetaldehyde;
目 录
1 前言 1
1.1 背景 1
1.1.1 食品香精香料 1
1.1.2 呋喃类香料 2
1.1.3 分离方法 3
1.1.4 柱色谱分离技术 4
1.2 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛合成方法 4
1.2.1 6、7-环氧柠檬醛在乙腈 - 硫酸条件下重排 4
1.2.2 6,7-环氧柠檬醛在硅藻土存在条件下重排 5
1.3 我的合成路线 6
2 试剂与仪器 7
2.1 试剂 7
2.2 仪器 8
2.3 装置图 8
2.3.1 还原反应装置图 8
2.3.2 旋转蒸发仪装置图 9
2.3.3 柱层析装置图 10
3 实验步骤 12
3.1 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛的制备 12
3.2 粗产物的后处理 12
3.2.1 调节PH值 12
3.2.2 萃取 12
3.2.3 干燥 12
3.2.4 旋转蒸发 12
3.2.5 点板 13
3.2.6 柱层析 13
4 结果与讨论 14