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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[1~3]报道的高。
The compound 6,7-difluoro-1-methyl-4-oxo-4H- [1,3] thiazino [3,2-a] quinoline-3-carboxylate was reacted with tris Acetylboron oxide chelated in DMSO to prepare the key intermediate of prulifloxacin 6,7-difluoro-1-methyl-4-oxo-4H- [1,3] thiazino [3,2 -a] quinoline-3-carboxyl-O6, O7-diacetate boron, different solvents were investigated, the reaction temperature and reaction time of 6,7-difluoro-1-methyl-4-oxo-4H- [ 1,3] thiazino [3,2-a] quinoline-3-carboxy-O6, O7-diacetate boron yield. The results showed that the mass fraction of the product was up to 99.8% (HPLC normalization), the yield was 97.1%, and the mass fraction and yield were higher than those reported in literatures [1-3].