Study on preparation method of reference substance of aristolactam Ⅰ-deoxyriboside adducts
A two-step synthetic process of bromination and cross-coupling with aristololactam Ⅰ as raw material was successfully developed.Three aristolactam Ⅰ-deoxyriboside adducts,namely AAⅠ-dA,AAⅠ-dG,and AAⅠ-dC were obtained after a sequential procedure of impurity removal and purification in four different solvents.The yield of the two-step reaction can reach 90%,and the pu-rity of the product is more than 98%,which can meet the requirements of qualitative and quantitative analyses as traditional Chinese medicine chemical reference products.The process has been proven to have good repeatability and scalability,and it features a concise preparation procedure,efficient purification,and high yield and purity,requiring no chromatographic separation.Compared with pre-vious methods,the newly developed process has significant advantages and is suitable for the preparation of chemical reference products of aristolactam Ⅰ-deoxyriboside adducts.This process provides technical support for the preparation of reference products of aristolac-tam Ⅰ-deoxyriboside adducts and a solid material basis for the related toxicological research.
aristolactam Ⅰ-deoxyriboside adductssynthesis and preparationbromination reactioncoupling reaction
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