药学专业毕业论文--5-氨基邻甲酚的制备及研究
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摘 要 5-氨基邻甲酚具有抗肿瘤作用，其主要用途是作为染发剂中间体。目前，在欧洲和日本5-氨基邻甲酚均有一定的市场，但在国内还少有厂家生产。 本文以大红色基G通过在冰水浴和稀硫酸条件下进行重氮化，制得重氮盐。重氮盐在较浓硫酸和一定温度条件下进行水解反应得到5-硝基邻甲酚。5-硝基邻甲酚在稀酸条件下，与还原铁粉进行还原反应，将硝基还原成氨基，从而得到5-氨基邻甲酚。 本文主要考察了合成5-硝基邻甲酚和5-氨基邻甲酚所需的条件。其中通过对5-硝基邻甲酚制备过程中水解时间，水解温度和硫酸浓度对5-硝基邻甲酚的产率的考察，从而确定了5-硝基邻甲酚制备时所需的最优条件分别为水解时间1.5h和水解温度为80℃，硫酸浓度则是在一定范围内浓度越高5-硝基邻甲酚的产率越高。对5-氨基邻甲酚的制备过程中，随着5-硝基邻甲酚用量的增加5-氨基邻甲酚的产率也是稳定增加，说明了很好的工艺放大性。 关键词：5-硝基邻甲酚；5-氨基邻甲酚；重氮化；染发剂；硝基还原 Title Preparation and Study of 5 - Amino-o-cresol 1 Abstract 5 - Amino-o-cresol is with anti-tumor effect, and its main use is as a hair dye intermediate. Currently, in Europe and Japan 5 - amino-o-cresol have a certain market, but there is little in the domestic manufacturers. In this paper, in the ice water bath and dilute sulfuric acid conditions, the 4 - nitro -2-diaminotoluene diazotization obtained diazonium salt. Under the conditions of a certain temperature and doctrinal concentration of sulfuric acid, through hydrolysis reaction, diazonium salt produce 5-nitro-o-cresol. In acid conditions, 5 - nitro-o-cresol and reduced iron powder by reduction reaction, the reduction of nitro into amino acids, which produce 5 - amino-o-cresol. This paper investigated the required composite conditions of 5 - nitro-o-cresol and 5 - amino-o-cresol. Through the study of 5-nitro-o-cresol yield influencing factors, which include the hydrolysis time, hydrolysis temperature and sulfuric acid concentration, we can determine the optimal conditions of the 5-nitro-o-cresol needed. namely, hydrolysis time 1.5h and the hydrolysis temperature is 80 ℃. Within a certain range, the higher the concentration of sulfuric acid the more high yield. In the preparation process of 5-amino-o-cresol, with the amount of the 5-nitro-o-cresol increasing, the yield of 5-amino-o-cresol also steady increase. This shows a good amplification of the process. Keywords 5-nitro-o-cresol, 5-Amino-o-cresol, Diazotization, Hair dye, Nitro reduction 2 目 次 1 前言 ............................................................ 4 1.1 染发剂的定义及分类 .......................................... 4 1.1.1 暂时性染发剂 ......................................... 4 1.1.2 半永久性染发剂........................................ 4 1.1.3 永久性染发剂.......................................... 4 1.2 染发剂的毒性作用 ............................................ 5 1.3 5-氨基邻甲酚的理化性质及用途 ................................ 5 1.4 5-氨基邻甲酚现有的合成方法[2] ................................ 5 1.4.1 氯化法................................................ 5 1.4.2 磺化法................................................ 6 1.4.3 硝化法................................................ 6 1.4.4 重氮法................................................ 6 1.5 5-氨基邻甲酚的合成原理的选择 ................................ 7 1.6 本课题的目的及意义 .......................................... 7 2 实验部分 ......................................................... 8 2.1 实验试剂及仪器 .............................................. 8 2.1.1 仪器.................................................. 8 2.1.2 试剂.................................................. 8 2.2 实验步骤 .................................................... 9 2.3 实验结果及讨论 ............................................. 12 2.3.1 水解反应中温度对产物5-硝基邻甲酚的影响 ............... 12 2.3.2 水解反应中硫酸浓度对产物5-硝基邻甲酚的影响 .......... 12 2.3.3 水解时间对中间产物5-硝基邻甲酚的影响 ................ 13 2.3.4 水解过程中不同加料方式对5-硝基邻甲酚产率的影响 ...... 14 2.3.5 5-氨基邻甲酚的工艺放大实验........................... 15 2.3.6 还原过程后含水量对5-氨基邻甲酚产率的影响 ............ 15 2.4 红外光谱分析 ................................................ 16 2.4.1 5-硝基邻甲酚的红外分析............................... 16 2.4.2 5-氨基邻甲酚的红外分析............................... 17 结 论 ............................................................. 18 致 谢 ............................................. 错误!未定义书签。 参 考 文 献 ....................................................... 19 3 本文来源：https://www.wddqw.com/doc/2bf9b714baf67c1cfad6195f312b3169a551ea5e.html