| 第 47 卷第 1 期 |  | Vol. 47 No. 1 | | 2017 年 2 月 | Feb 2017 |
|
所屬欄目：醫藥及中間體
一種德拉沙星的制備方法 |
| 王秀娟，郭彥玲
（魯南制藥集團，山東 臨沂 276002） |
| 摘 要：以2，4，5-三氟苯甲酰乙酸乙酯為起始物，經(jīng)縮合、氯代、水解制得德拉沙星，其中氯代反應考察了提純方法，使5位氯代物雜質(zhì)減少；水解反應優(yōu)化水解條件，使氧化雜質(zhì)減少。用該方法制得的德拉沙星純度大于99.8%，5位氯代雜質(zhì)和氧化雜質(zhì)均小于0.1%，滿(mǎn)足藥用要求。操作簡(jiǎn)單，對設備無(wú)苛刻要求，具有工業(yè)化應用前景。 |
| 關(guān)鍵詞：德拉沙星；2，4，5-三氟苯甲酰乙酸乙酯；5位氯代雜質(zhì)；氧化雜質(zhì) |
| 中圖分類(lèi)號：0625.2 文獻標識碼：A 文章編號：1009-9212（2017）01-0056-04 |
|
| Preparation of Delafloxacin |
| WANG Xiu-juan, GUO Yan-ling
(Lunan Pharmaceutical Group Corporation, Linyi 276002, China) |
| Abstract：This article reported a method for the preparation of Delafloxacin, which had advantages including simple operation-process, no rigid requirements for equipment, high yield and high purity of final product. All advantages made this method suitable for industrial production. In this method, ethyl 2,4,5-trifluorobenzoylacetate was selected as the starting material, and the final product was obtained through reactions including condensation, chlorination, hydrolysis. In the manufacturing process, the purification method for chlorination had been studied to reduce 5-chlorinated impurity, meanwhile, the conditions for hydrolysis had been optimized to reduce the amount of oxidant. Through all of the improvements, Delafloxacin obtained in this method had very high quality with a purity more than 99.8%, both 5-chlorinated and oxidant impurity were less than 0.1%. |
| Key words：Delafloxacin; ethyl 2,4,5-trifluorobenzoylacetate; 5-chlorinated impurity; oxidant impurity |
|
作者簡(jiǎn)介：王秀娟（1980-），女，山東濰坊人，工程師，研究方向：藥物研發(fā)（E-mail:xiujuan0103@163.com）。
|
收稿日期：2017-02-13
|
|