普卢利沙星关键中间体的合成研究  

Study on Synthesis of the Key Intermediate of Prulifloxacin

作　　者：郝二军[1] 程传玲[2] 徐桂清[1] 李伟[1] 胡志国[1] 渠桂荣[1] 

机构地区：[1]河南师范大学化学与环境科学学院,河南新乡453002 [2]郑州轻工业学院食品与生物工程学院,河南郑州450002

出　　处：《精细化工》2009年第10期996-998,共3页Fine Chemicals

基　　金：国家自然科学基金项目(20473026)~~

摘　　要：用螯合法把化合物6,7-二氟-1-甲基-4-氧代-4H-[1,3]噻嗪并[3,2-a]喹啉-3-羧酸乙酯与三乙酰氧化硼在DMSO中螯合,制得普卢利沙星的关键中间体6,7-二氟-1-甲基-4-氧代-4H-[1,3]噻嗪并[3,2-a]喹啉-3-羧基-O6,O7-二乙酸合硼,考察了不同溶剂、反应温度、反应时间对6,7-二氟-1-甲基-4-氧代-4H-[1,3]噻嗪并[3,2-a]喹啉-3-羧基-O6,O7-二乙酸合硼收率的影响。结果表明,所得产物的质量分数可达99.8%（HPLC归一法）,产率97.1%,质量分数和产率都比文献报道的高。A novel synthetic route of 5,6-difluoro-1-methyl（-4-oxo-4H-thiazeto-quinoline-3-carboxylic-O6,O7-boron diethyl carboxylate（Ⅰ） was designed.The synthesis of（Ⅰ） from 5,6-difluoro-1-methyl（-4-oxo-4H-thiazeto-quinoline-3-carboxylic acid ethyl ester was performed by means of the Borlc coordination complex in this paper.The target compound was obtained by the Chelated Method.The reaction yield in different solvents,at different reaction temperatures and time were discussed in this paper.DMSO was finally used.The neutral titration was considered to be the best method in the hydrolysis reaction of the condensation product. The total yield was 97. 1%.

关 键 词：6 7-二氟-1-甲基-4-氧代-4H-[1 3]噻嗪并[3 2-a]喹啉-3-羧基-O6 O7-二乙酸合硼 硼螯合物 普卢利沙星 医药与日化原料 

分 类 号：R927.2[医药卫生—药学]