摘要:使用6,6’-二甲基-2,2’-联吡啶-4,4’-二甲酸为原料,先通过酯化反应得到酯,然后通过过氧剂的氧化反应得到相应的氮氧化物,由氮氧化物与醋酸酐反应得到相应的环合产品“6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯”。这一次论文要进行实验得到进一步优化的反应过程条件,然后在此条件下,合成出合格的产品,并对产品进行相应的分析与鉴定。在实验中要考察不同相转移催化剂,催化剂的用量及能否可以循环使用,反应温度,反应时间,不同的强酸及其用量对反应的影响;得到最优反应条件.68807
毕业论文关键词: 6,6’-二甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯;中间体
6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯
Preparation of dimethyl 6,6'-diacetoxymethyl-2,2'-bipyridine-4,4'-dicarboxylate
Abstract: The esterification reaction is carried out by using 6,6'-dimethyl-2,2'-bipyridyl-4,4'-dicarboxylic acid as raw material, and then the corresponding nitrogen oxides are obtained by the oxidation reaction of the peroxide , By the reaction of nitrogen oxides and acetic anhydride to get the corresponding cyclization product 6,6'-diacetoxymethyl -2,2'-bipyridyl-4,4'-dicarboxylate. In this paper, the optimal reaction conditions are obtained through experiments, and then under this condition, the qualified products are synthesized and the products are analyzed and identified accordingly. In the experiment, the effects of different phase transfer catalyst, catalyst dosage and the ability of recycling, reaction temperature, reaction time, different strong acid and its dosage on the reaction were investigated. The optimum reaction conditions were obtained.
Key Words: Voriconazole; 6-ethyl-5-fluoro-4-hydroxypyrimidine; prepare process intermediates
目录
1绪论 1
1.1 6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯的概述 1
1.2 6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯的国内外研究现状 4
1.3 6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯的市场前景 6
1.4 本课题主要研究内容 7
2 6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯的制备 7
2.1 拟使用的材料试剂、仪器设备 7
2.1.1 试剂药品 7
2.1.2 仪器设备 8
2.2 6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯的合成 9
2.2.1 实验前的预处理 9
2.2.2 6,6’-二甲基2,2’-联吡啶-4,4’-二甲酸二甲酯的制备 10
2.3 6,6-二甲基-2,2-联吡啶基-4,4-二羧酸酯的制备 11
2.3.1 6,6-二甲基-2,2-联吡啶基-4,4-二羧酸酯的合成方法 11
2.3.2 制备实验过程 12
2.4 6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯的制备 12
2.4.1 6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯的合成方法 12
2.4.2 6,6’-二乙酰氧基甲基-2,2’-联吡啶-4,4’-二甲酸二甲酯的具体实验步骤