氟哌酸合成工艺优化

文档编号:ZY100    文档字数:6477,页数:18

摘要：氟哌酸是第三代喹诺酮类抗菌药物的优秀代表之一, 它的合成路线有很多种，而以形成硼螯合物的方法倍受关注。中间体(1-乙基-6-氟-7-氯-1,4-二氢-4-氧代-喹啉-3-羧酸-O3O4)-二-(乙酸-O)-硼与哌嗪的缩合反应是氟哌酸生产工艺中的关键步骤。本文档用正交试验法对氟哌酸缩哌反应条件进行了优化设计。通过考察缩哌反应的反应温度、反应时间、反应物的配料比和溶剂的用量等四种因素，用L16(44)正交试验筛选得出该反应的最佳工艺条件为：反应温度70℃，反应时间6h，无水哌嗪:螯合物摩尔比=4:1，溶剂使用量甲苯:DMF质量比=50:20。

关键词：氟哌酸；无水哌嗪；缩合；正交设计

Abstract: Norfloxacin is one of the outstanding representatives of the third generation of quinolone antibiotics，and there are a good deal of methods for synthesizing it. Forming boride is the most useful method. Piperazine condensation of intermediate (1-ethyl-6-fluoride-7-chloro-1,4-dihydro-4-oxo-
quinoline-3-carboxylic acid-O3O4)-bis-(acetate-O)-boron is a crucial step in norfloxacin production. Optimizing the best conditions of piperazine condensation by orthogonal test. Reaction temperature, time, reactant mixture ratio and the amount of solvent were discussed. The best condition of piperazine condensation was investigated by L16(44) orthogonal design. At the temperature of 70℃, 6 hours, molar ratio of anhydrous piperazine : chelate complex = 4:1, dosage of solvents toluene : DMF = 50 : 20 by mass ratio are the best conditions.

Key words: Norfloxacin; Anhydrous piperazine; Condensation; Orthogonal design

目  录
中文摘要 I
英文摘要 II
目录 III
1. 绪论 1
 1.1 前言 1
 1.2 研究现状 1
2. 实验部分 5
 2.1 实验仪器和试剂 5
 2.1.1 实验仪器 5
 2.1.2 实验试剂 5
2.2 实验操作步骤 5
3. 结果与讨论 8
 3.1 正交实验方案设计 8
3.2 实验结果数据处理 9
4．总结与展望 12
 4.1 总结 12
 4.2 展望 12
致谢 14
参考文献 15

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