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摘要本论文研究了用亚硝酸甲酯作为重氮化试剂来合成三氮烯类化合物和偶氮类化合物的研究。具体内容如下：首先通过对绿色化学和重氮化方法绿色改进的综述，用亚硝酸甲酯作为重氮化试剂来进行重氮化反应合成三氮烯类化合物的研究。用盐酸、亚硝酸钠和甲醇制备的亚硝酸甲酯作为重氮化试剂，过程中没有二氧化氮、一氧化氮等气体的产生，副反应少，产率高。其次，亚硝酸甲酯重氮化反应合成一般偶氮类化合物的研究。用亚硝酸甲酯在低温的条件下制备重氮盐，不经处理，直接进入后续的偶联反应。不仅优化了实验操作的简便性，而且通过控制反应溶液的pH值，不需要进一步纯化就可以拿到反应的产物，符合绿色合成发展的需要。第三，磺酸类偶氮化合物的绿色合成的研究。用亚硝酸甲酯和对氨基苯磺酸制备重氮盐，接着用制得的重氮盐与芳胺或者酚类化合物进行偶合反应来合成带有磺酸基的偶氮化合物。反应结束后通过反应pH值的控制，不需要进一步的分离，就可以得到相应的产物，实验操作简单，后处理方便。用亚硝酸甲酯制备上述化合物的反应条件温和、过程环保、操作简单。48326
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In this dissertation, synthesis of triazenes and diazo-compounds by using methyl nitrite were investigated. Firstly, synthesis of triazene compounds using methyl nitrite as a diazotization reagent was produced by hydrochloric acid with sodium nitrite and methanol, through review of the Green Chemistry and the improvement of the diazotizatization methods. It has no nitric oxide and nitrogen dioxide were produced and less side reactions and good yield in this process. Secondly, synthesis and studies of the general diazo-compounds by using methyl nitrite. The diazonium salts were produced by methyl nitrite under low temperature and straightly used in the coupling reactions. It is not only make the operation easy, but also can obtain the produces without prorification by controlling the pH of the reaction mixture. This is consistent with Green Chemistry. Thirdly, Green synthesis and studies of azo compounds containing sulfo functional group were synthetized by aromatic amines or phenols and diazonium salt produced by the reaction of para-aminophenylsulfic acid with methyl nitrite. The produces can be obtained without further isolation. It is easy to manipulate and post process. The evident advantages of the method for preparation of the above compounds are mild reaction conditions, good yields, environmental benign, and easy to work up.
毕业论文关键词：绿色化学；重氮化；亚硝酸甲酯；三氮烯；偶氮化合
Keyword: Green Chemistry；diazotization；methyl nitrite；triazene；azo-compound
目 录
引言 4
1.实验背景概述5
1.1 三氮烯化合物的性质与应用•5
1.2 偶氮类化合物的性质与应用•6
1.3 磺酸类偶氮化合物的性质与应用•7
2.实验部分9
2.1 实验试剂和仪器•9
2.1.1 实验仪器•9
2.1.2 实验试剂10
2.2 实验过程10
2.2.1 亚硝酸甲酯的制备10
2.2.2 三氮烯类化合物的制备10
2.2.3 偶氮类化合物的制备11
2.2.4 磺酸类偶氮化合物的制备13
2.3 实验结果15