克林霉素磷酸酯中有机溶剂残留量的毛细管顶空GC测定

A capillary GC method with headspace was established for determination of residual organic solvents——ethanol, propanone, dichloromethane, chloroform and pyridine in clindamycin phosphate. A DB-624 capillary column wasused with water as the solvent. The average recoveries of the five solvents were 98.2%, 96.7%, 98.6%, 97.5% and 103.1%,respectively. The detection limits were 7.8, 3.8, 0.4, 0.6 and 2.0μg/ml, respectively.

氟罗沙星的合成

以 6 ,7,8-三氟 - 1,4 -二氢 - 4 -氧代 - 3-喹啉酸乙酯为原料 ,经氟乙基化、与 N-甲基哌嗪缩合和水解等 3步反应制得氟罗沙星 ,总收率 6 7.5 %。工艺操作简单 ,适于工业生产。

呱氨托美丁合成工艺的改进

以托美丁钠为起始原料,与氯甲酸异丁酯、甘氨酸反应生成中间体托美丁甘氨酰胺,再与氯甲酸异丁酯、愈创木酚反应制得呱氨托美丁,同时对其的精制方法进行了研究。结果显示:改进后的工艺反应条件温和,操作简单,提高了目标物的质量,总收率65%,具有较大的产业化生产优势。