Separation and identification of an impurity from the istradefylline intermediate,RSC Advances

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Separation and identification of an impurity from the istradefylline intermediate
RSC Advances ( IF 3.9 ) Pub Date : 2020-4-8 , DOI: 10.1039/c9ra09074f
Haojie Xu _{1,

2} , Yiyun Wang _{1,

2} , Hongyi Wang _{1,

2} , Zhonghui Zheng ₂ , Zihui Meng ₁ , Min Xue ₁ , Zhibin Xu ₁

Affiliation

Istradefylline is a selective adenosine antagonist for the A_2a receptor, and it is used to treat the Parkinson's disease and improve dyskinesia in the early stage of the Parkinson's disease. An impurity in the istradefylline intermediate A₁ (6-amino-1,3-diethyl-2,4-(1H,3H)-pyrimidinedione) was identified by high performance liquid chromatography (HPLC); it was separated by preparative HPLC and further characterized by UV, IR, MS, NMR, 2D NMR and single-crystal XRD analyses. The impurity was identified as (E)-N-ethyl-2-cyano-3-ethylamino-2-butenamide, which originated from the synthetic process of the intermediate A₁. The structure of this impurity might affect the efficiency and safety of istradefylline; therefore, the research and control of this impurity are necessary for ensuring the quality of istradefylline.

中文翻译：

从伊曲茶碱中间体中分离和鉴定杂质

Istradefylline是A _2a受体的选择性腺苷拮抗剂，用于治疗帕金森病和改善帕金森病早期的运动障碍。异曲茶碱中间体A ₁（6-氨基-1,3-二乙基-2,4-(1 H ,3 H )-嘧啶二酮）中的杂质通过高效液相色谱（HPLC）鉴定；通过制备型 HPLC 对其进行分离，并通过 UV、IR、MS、NMR、2D NMR 和单晶 XRD 分析进一步表征。该杂质经鉴定为( E ) -N-乙基-2-氰基-3-乙基氨基-2-丁烯酰胺，来源于中间体A _{1的合成过程}. 这种杂质的结构可能会影响伊曲茶碱的有效性和安全性；因此，该杂质的研究和控制对于保证伊曲茶碱的质量是必要的。

更新日期：2020-04-08

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