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摘要：论文的主要目标是研究2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醇的分离提纯。其中2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醇是2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛以硼氢化钠作为还原剂还原得到。在该还原过程中会有2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醇的同分异构体和其它一些副产物产生。因此，这些物质都会对目标产物的分离提纯产生影响。我在本试验中采用的分离方法主要有：萃取、干燥、旋转蒸发、柱层析等。其中柱层析是我分离提纯的主要手段。在该过程中，采用硅胶作为固定相，以不同配比的乙酸乙酯和石油醚作为展开剂。采用薄层分析的方法对分离出的产物作初略鉴定。对鉴定出的目标产物进行合并收集，并对收集的组分进行核磁共振氢谱、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55%左右。43674
毕业论文关键词：还原反应；2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醇；柱层析；薄层色谱法
2- (5- (2-hydroxy-2-yl) -2-methyl-tetrahydrofuran-2-yl) ethanol Separation and purification
Abstract: The objective of this paper is to study the separation and purification of 2- (5- (2-hydroxy-2-yl)-2-methyl-tetrahydrofuran-2-yl) ethanol and identify .The 2- (5- (2-hydroxy-2-yl)-2-methyl-tetrahydrofuran-2-yl) acetaldehyde is reduced by
sodium borohydride . The isomers of 2- (5- (2-hydroxy-2-yl)-2-methyl-tetrahydrofuran-2-yl) ethanol is produced in the process of the reduction. There are still some by-products. As a result, these substances will have a negative effect of the separation. The separation methods used in this experiment are extraction, rotary evaporation, column chromatography, etc. The column chromatography separation and purification is my main means. The stationary phase is silica and the mobile phase is made by different ratio ethyl acetate and petroleum ether. The final target product is collected to analyze by nuclear magnetic resonance hydrogen spectrum, infrared spectrum and gas chromatography-mass spectrometry. According to the results, the yield is about 55%.
Keywords: reduction reaction; 2- (5- (2-hydroxy-2-yl)-2-methyl-tetrahydrofuran-2-yl) ethanol; column chromatography ; column chromatography; thin-layer chromatography
目录
1 前言 1
1.1 背景 1
1.2 合成方法 2
1.2.1 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛的合成 2
1.2.2 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醇的合成 3
1.3分离提纯方法 3
2 试剂与仪器 6
2.1 试剂 6
2.2 仪器 7
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 8
2.3.3 柱层析装置图 9
3 实验步骤 11
3.1 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醇的制备 11
3.2 产物的后处理 11
3.2.1 调节PH值 11
3.2.2 萃取 11
3.2.3 干燥 11
3.3 硅胶柱法分离提纯粗产物