摘要
研究一种制备甲磺酸达氟沙星N-脱甲基杂质标准品的方法。以甲磺酸达氟沙星为起始原料,通过碘氧化实现N-脱甲基反应,随后进行精制和后处理步骤,最终获得含量97.13%(HPLC)的目标杂质标准品N-脱甲基。方法操作简便且产物纯度高,其结构经^(1)H NMR、HRMS等确证。
This research is to develop a method for preparing N-demethylated impurity reference standards of Dafloxacin Mesylate.This method uses Danofloxacin Mesylate as the initial raw material,it also utilized iodinemediated oxidation to carry out the demethylation reaction.Following this,refinement and post-processing steps are conducted to reach a target for impurity reference standards N-demethyl at 97.13%(HPLC).The advantages of this approach lie in its simplicity of operation and the high purity of the product,with the structure confirmed by techniques such as ^(1)H NMR and HRMS.
作者
单国洋
黄秋波
许培德
曹勇
凃鑫
SHAN Guo-yang;HUANG Qiu-bo;XU Pei-de;CAO Yong;TU Xin(Zhejiang Guobang Pharmaceutical Co.,Ltd.,Shangyu 312369,China)
出处
《精细化工中间体》
CAS
2024年第3期52-54,共3页
Fine Chemical Intermediates
关键词
达氟沙星
N-脱甲基杂质
合成
Danofloxacin
N-demethylated impurities
synthesis
