酒石酸唑吡坦片中2种杂质的合成

Synthesis of Two Kinds of Impurities in Zolpidem Tartrate Tablets

目的:设计合成酒石酸唑吡坦片中杂质Ⅰ。方法:以唑吡坦及1-溴代乙酸乙酯为起始原料,经一锅法合成得到酒石酸唑吡坦片中的杂质Ⅰ(4-(二甲胺基)-3-(6-甲基-2-对甲苯基咪唑并[1,2-a]吡啶-3-基)-4-氧代丁酸),同时杂质Ⅱ(2-羟基-N,N-二甲基-2-(6-甲基-2-对甲苯基咪唑并[1,2-a]吡啶-3-基)乙酰胺)作为副产物被合成得到。结果:成功获得酒石酸唑吡坦的两个新杂质,纯度分别为95.3%及97.2%,并经质谱和核磁共振(MS,1H NMR)进行结构确证。结论:首次合成了杂质Ⅰ及杂质Ⅱ,可为酒石酸唑吡坦质量控制和工艺优化提供参考依据。

Objective： To design and synthesize impurity Ⅰ in zolpidem tartrate tablets. Methods： Zolpidem and ethyl bromoacetate were used as the starting materials to synthesize impurity Ⅰ by a one-pot reaction,and impurity Ⅱ was obtained as a by-product.Results： The target compounds were synthesized,and characterized by MS and1 H NMR. And the purity was 95. 3% and 97. 2%,respectively. Conclusion： The impurity Ⅰ and impurity Ⅱ are synthesized for the first time,which can provide scientific information for the quality control and process optimization.