对甲基儿茶酚二乙酸二甲酯的合成研究-化学工艺专业论文.docxVIP

PAGE PAGE 5 摘要 本文总结了对军基儿茶勤及对甲基 JL茶酷二乙酸二叩酶的文献合成方法， 从 中筛选出了一条以对甲酸为起始原料的合成路线，经乙商在化、重排、达金氧化 及隧化反应，制得目标产物对甲基儿茶酸二乙酸二甲醋。本文合成产物主要作为 抗菌素、氧化拇制剂、受体兴奋剂以及支气管扩张剂的药物中间体。出外商委托 开发。 在合成对甲慕儿茶盼的工艺研究过程中，通过对每一步反应的不同物料配 比变化、温度变化、反应时间变化的研究，找出一条较适合工业化生产的优化工 艺路线F 对达金氧化反应的非均相氧化反应法和均相氧化反应法进行了比较研 究，得出了均相氧化反应法选择性好，转化率高的结论，同时对乙欧化反应和达 金氧化反应的催化剂的使周也进行了研究。对甲荔儿茶盼的收率在 88% 以上。 在合成对职基 JL茶盼二乙酸二甲酶的研究过程中啻对 一步反应法和两步反应法进 行了比较研究，考虑到生产成本及设备等因素，最后选择了一步反应法。收率超 过 80%。夜整个实验研究过程中，通过对每一步反应不同工艺条件的多方面改进 以及对比摸索步确定了一条较为科学的合成工艺路线，为工业化生产奠定了坚实 的基础。 关键词对申可对原基 7:云盼对甲基儿茶盼二乙酸虽醋乙散石室排 求 达?化号均吧非均吵 ABSTRACT Various synthetic methods of p-Methylca加chol and p-Methylcatechol dimethylacetate are reviewed. A commerciatly economic process is obtained for preparation of p-Methylcatechol and p-Methylcatechol dimethytacetate from 队Creso) by acetylization ， Freis rearrangement ， Dakin H 0 oxìdation and etherification. These ∞mpounds are useful as intermediates in preparation of pharmaceutically active ∞mpounds such as anti-bacterials ，COCαdioststs and antioxidants. During preparation of 4-Methylcatechol ，a suitable industrial帽scale production process is designed from the study of the change the materials ratio，the reaction temperature and reaction time for every step of reactions. Homogeneous Dakin H 0 oxìdatìon reaction can get higher yield and percent conversion ∞mpare wìth heteroegeneous Dakin H 0 oxidation reaction. 了he catalysts are also very important during the reaction of acetylization and Dakin H o oxidation. It was showed that the yield was more than 88%了he preparation of p-Methylcatechol dimethyface组te by the reaction of p-Methytcatechol and Methyl chloroacetate or p-Methylcatechol and Chloroacetic acid and Methyl alcohol. The one step reactíon is be枝er for industrial-scale production. The yield was over 80%. In the course of experiment ，by improving and investigating technical conditions of each step of reactions ， a scientific synthetic route and a favourable techni创 conditions have been