2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛的脱水反应研究

摘要：本文旨在研究2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛在酸的条件下反应，得出的脱水产物的结构式。在实验中，我们选取了50％的硫酸作为脱水反应的酸，与之进行脱水反应。将2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛m=0.5g，和8mL的50％的硫酸在室温下稍微加热，并使两者搅拌回流16h左右，使之进行充分的脱水反应，再用15mL的正己烷进行萃取，饱和的碳酸氢钠溶液和氯化钠溶液洗涤，再用无水硫酸钠干燥，等翌日再进行过滤浓缩等步骤，得到比较纯的产物。通过运用气相色谱-质谱联用仪，作出气相色谱图和质谱图，但最终的脱水产物并非文献上的理论产物，经过分析，脱水产物是2，6-二甲基-2-庚烯-5-酮醛。根据计算得出，2，6-二甲基-2-庚烯-5-酮醛的质量为0.34g。57607

毕业论文关键词： 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛；脱水反应；50％硫酸；2，6-二甲基-2-庚烯-5-酮醛

The research of 2-(5-(2-hydroxy propyl-2-yl) -2- methyl tetrahydrofuran-2-yl) acetaldehyde dehydration reaction

Abstract: This passage mainly to study 2-(5-(2-hydroxy propyl-2-yl)-2- methyl tetrahydrofuran-2-yl) acetaldehyde dehydration in acid under the conditions of the reaction, it is concluded that the formula of dehydration product . In the experiment, we selected the 50% sulfuric acid as acid dehydration reaction, and the dehydration reaction. 2-(5-(2- hydroxy propyl-2-yl)-2- methyl tetrahydrofuran-2-yl) acetaldehyde m = 0.5 g, and 8 ml of 50% sulfuric acid at room temperature, a little heat, and make the two mixing reflow 16 hours or so, to fully dehydration reaction, with 15 ml of normal hexane extraction, saturated sodium bicarbonate solution and sodium chloride solution of washing, dry with anhydrous sodium sulfate, filtered again the next day, the next day，making concentration and other steps, to get more pure product. By gas chromatography - mass spectrometry chromatography。But in the end product dehydration is not reported in the literature theory, through analysis, but the dehydration product is m/z = 154 ,the name is 2, 6 - dimethyl -2- heptene -5- ketone aldehyde.According to the calculated, the quality of 2, 6 - dimethyl - 2 - heptene - 5 - ketone is 0.34 g.

Keywords:2-(5-(2-hydroxy-2-yl)-2-methyl-tetrahydrofuran-2-yl) acetaldehyde;dehydration reaction；50% sulfuric acid；2, 6- dimethyl -2- heptene -5- ketone aldehyde.

1 前言 5

1.1 背景 5

1.1.1 四氢呋喃 5

1.1.2 PTSA 6

1.1.3 四氢呋喃类香料 6

1.1.4 醚类香料 7

1.2 6,7-柠檬醛的重排 8

1.2.1 6,7-环氧柠檬醛在硅藻土存在条件下重排 8

1.2.2 6,7-环氧柠檬醛在稀H2SO4条件下与丙酮缩合 9

1.2.3 7-环氧柠檬醛在乙腈-硫酸条件下重排 9

1.3 我的合成路线 10

1.3.1合成方法 10

1.3.2 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛的脱水反应 11

2 试剂与仪器 12

2.1 试剂 12

2.2 仪器 12

2.3 装置图 13

3 实验步骤 14

3.1 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛的脱水反应 2-(5-(2-羟基丙-2-基)-2-甲基四氢呋喃-2-基)乙醛的脱水反应研究:http://www.youerw.com/huaxue/lunwen_62387.html