1-环丙基-6,7-二氟-8-甲氧基-1,4-二氢-4-氧代喹啉羧酸乙酯精制方法的考察

Study of the refining method of cyclopropyl-6,7-difluoro-8-methoxy-1,4-dihydro-4-oxoquinoline-3-carboxylate

目的 :采用不同溶剂重结晶法对 1-环丙基 - 6,7-二氟 - 8-甲氧基 - 1,4 -二氢 - 4 -氧代喹啉羧酸乙酯精制并对精制品进行质量分析 ,从而确定较理想的精制方法。方法 :采用无水乙醇、甲醇、乙酸乙酯、丙酮作为重结晶溶剂 ,采用熔点、红外光谱、高效液相色谱法对精制品进行质量分析。结果 :四种精制品的外观、熔点基本一致 ;IR光谱一致 ;纯度差异较大 ,丙酮精制品纯度为82 .4 % ,其余三种均大于 98%。结论 :选用无水乙醇进行精制 。

OBJECTIVE:Selecting a better refining method of 1 cyclopropy1 6, 7 difluoro 8 methoxy 1,4 dihydro 4 oxoquinoline 3 carboxylate (Ⅰ).METHOD:The refinement to (Ⅰ) used four kinds of solvent absolute ethanol,methanol,ethyl acetate and acetone.The analysis of it included melting point,IR and HPLC.RESULTS:The appearance and melting point of the four refined (Ⅰ) are similar.IR spectrum are the same,but the purity are different.CONCLUSION:The purity of (Ⅰ) was higher while (Ⅰ) was refined in absolute ethanol.