离子液体催化合成烯丙基缩水甘油醚的研究

摘要：本论文以吡啶、氯代正丁烷以及氟硼酸钠为原料，采用正交试验方法两步合成了离子液体N-丁基吡啶四氟硼酸盐，研究了不同反应条件对产物产率的影响，并通过IR和1H-NMR技术对所制备产物进行了结构表征。将N-丁基吡啶四氟硼酸盐作为催化剂，研究了其催化合成烯丙基缩水甘油醚的可行性，产物的结构用IR和1H-NMR表征。实验结果表明，在反应温度为80℃，反应时间为16 h，n（氯代正丁烷）：n（吡啶）=1:1，溶剂乙腈用量20 mL时，中间体氯化N-丁基吡啶的产率最高。中间体经过离子交换，得到N-丁基吡啶四氟硼酸盐，其最佳合成条件是n（氟硼酸钠）：n（氯化N-丁基吡啶）=1:1，反应温度40℃，反应时间22 h，溶剂丙酮用量30 mL。7792
关键词：正交试验；离子液体；N-丁基吡啶四氟硼酸盐；合成；烯丙基缩水甘油醚
Study on the synthesis of allyl glycidyl ether by ionic liquid
Abstract: The N-butyl pyridine tetrafluoroborate ionic liquid was synthesized by two steps with pyridine, N-butyl chloride and sodium tetrafluoroborate and by using orthogonal test method. The influences of different reaction conditions on the yield of product were investigated. The prepared product was characterized and confirmed by IR and 1H-NMR techniques. The feasibility of the catalytic synthesis of allyl glycidyl ether using N-butyl-pyridine tetrafluoroborate as catalyst was studied and the product was characterized and confirmed by IR and 1H-NMR. Experimental results showed that the yield of the intermediate N-butyl pyridine chloride was highest when the mole rate of N-butyl chloride and pyridine was 1:1, amount of solvent acetonitrile 20 mL at 80 ℃ reacting 16 hours. The N-butyl pyridine tetrafluoroborate was obtained by ion exchange of the intermediate and its optimal synthesis conditions were that the mole rate of sodium tetrafluoroborate and N-butyl pyridine chloride was 1:1, amount of solvent acetone 30 mL at 40 ℃ reacting 22 hours.
Key Words: Orthogonal test; Ionic liquid; N-butyl pyridine tetrafluoroborate; Synthesis; Allyl glycidyl ether
目录
1绪论   1
1.1 课题背景和意义   1
1.2 离子液体概述   1
1.2.1 离子液体的组成   1
1.2.2 离子液体的性质   2
1.2.3 离子液体的研究进展   4
1.2.4 离子液体的合成   5
1.2.5 离子液体在有机合成中的应用   6
1.3 烯丙基缩水甘油醚概述   7
1.3.1 烯丙基缩水甘油醚简介   7
1.3.2 烯丙基缩水甘油醚合成方法   7
1.4 本课题研究内容与要求   8
2实验部分   10
2.1 主要实验试剂及仪器   10
2.1.1 实验试剂   10
2.1.2 实验仪器   10
2.2 实验步骤   10
2.2.1 中间体氯化N-丁基吡啶的合成   10
2.2.2 N-丁基吡啶四氟硼酸盐的合成   12
2.2.3 烯丙基缩水甘油醚的合成   13
3结果与讨论   14
3.1 中间体氯化N-丁基吡啶最佳合成条件的确定   14
3.2 N-丁基吡啶四氟硼酸盐最佳合成条件的确定   15
3.3 烯丙基缩水甘油醚的结果分析   16
3.4 中间体氯化N-丁基吡啶的结构表征   16
3.4.1 红外光谱（IR）分析   16
3.4.2 核磁共振氢谱（1H-NMR）分析   17
3.5 N-丁基吡啶四氟硼酸盐的结构表征   18
3.5.1 红外光谱（IR）分析   18
3.5.2 核磁共振氢谱（1H-NMR）分析   19 离子液体催化合成烯丙基缩水甘油醚的研究:http://www.751com.cn/huaxue/lunwen_5871.html