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摘要本论文以 2,2,2’,2’-四甲基-5,5’-二硝基-5,5’-双(1,3-二氧杂环己烷)为原料，经水解反应合成 2,3-二羟甲基-2,3-二硝基-1,4-丁二醇，再分别与乙酸和丙酸反应得到2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四乙酸酯和2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四丙酸酯。结合反应机理讨论了影响水解、酯化反应的主要因素，并对单元反应各个因素进行了优化，获得最佳工艺条件。64333
实验表明，水解较优条件为：甲醇:盐酸为20:1（体积比），反应时间6h，温度55℃，收率93.3%；2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四乙酸酯较优条件为：2,3-二羟甲基-2,3-二硝基-1,4-丁二醇4g，乙酸12mL，苯55mL，对甲苯磺酸1g，75℃下分水回流8h，收率52.37％；2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四丙酸酯较优条件为：2,3-二羟甲基-2,3-二硝基-1,4-丁二醇4g，丙酸12mL，苯55mL，对甲苯磺酸1g，75℃下分水回流10h，收率50.28％。并用1H NMR和IR对目标产物结构进行了表征。
毕业论文关键词：2,3-二羟甲基-2,3-二硝基-1,4-丁二醇，2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四乙酸酯，合成，表征。
毕业设计说明书（论文）外文摘要
Title Study on esterification reaction of 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol
Abstract 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol was prepared from 2,2,2’,2’- tetramethyl-5,5’-dinitro-5,5’-Bis(1,3-dioxane) by hydrolysis reaction. Then it was esterified with acetic acid and propanoic acid. The main factors of hydrolysis and esterification reaction were discussed according to reaction mechanism. And the conditions of each unit reaction were optimized.
Optimal conditions of hydrolysis reaction were obtained as follows:
methanol to hydrochloric acid was 20:1, reaction temperature was 55℃,
reaction time was 6h, the yield was 93.3%. Optimal conditions of 2,3-bis(hydro-xymethyl)-2,3-dinitro-1,4-butanediol tetraacetate were obtained as follows: 2,3- Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol 4 g, acetic acid 12 mL, benzene 55 mL, p-toluenesulfonic 1g, reacted 8h under 75℃, the yield was 52.37%. Optimal conditions of 2,3-bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol tetrapropi-onate were obtained as follows: 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanedi-ol 4g, benzene 55mL, propanoic acid 12mL, p-toluenesulfonic 1g, reacted 8h under 75℃, the yield was 50.28%. The product was characterized by melting point, 1H NMR, IR.
Keywords: 2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol; 2,3-bis(hydroxymeth-yl)-2,3-dinitro-1,4-butanediol tetraacetate; 2,3-bis(hydroxymethyl)-2,3-dinitro-1,4- butanediol tetrapropionate; synthesis, characterization
1 引言 1
1.1概述 1
1.1.1 课题背景 1
1.1.2 2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四酯的性质与用途 3
1.2 多元醇酯合成方法简述 3
1.2.1 酯化方法 3
1.2.2 酯化反应催化剂的选择 4
1.3 本文提出的2,3-二羟甲基-2,3-二硝基-1,4-丁二醇四酯的合成方法 5
1.4 本文主要内容 5
2 2,3-二羟甲基-2,3-二硝基-1,4-丁二醇的合成 6
2.1 反应式 6
2.2 反应原理 6
2.3 实验部分 7
2.3.1 实验仪器 7