降糖药达格列净中2种杂质的合成  

Synthesis of Two Impurities in Dapagliflozin

作　　者：王彪[1] 曹胜[1] 杜月[1] 李育芯 吴妹卿 胡春[1] 

机构地区：[1]沈阳药科大学基于靶点的药物设计与研究教育部重点实验室,辽宁沈阳110016

出　　处：《精细化工中间体》2016年第3期24-27,共4页Fine Chemical Intermediates

基　　金：国家"重大新药创制"科技重大专项(2009ZX09301-012)

摘　　要：为定量控制降糖药达格列净中的杂质,对达格列净中的2个杂质5-溴-2-氯-2′-乙氧基二苯甲酮(1)和5-溴-2-氯-2′-乙氧基二苯甲烷(2)进行了定向合成,以5-溴-2-氯苯甲酸和苯酚经缩合、Fries重排,然后乙基化得到杂质1,杂质1再经还原得到杂质2。其结构经核磁共振氢谱和质谱确证结构。To perform the quality control of dapagliflozin, two impurities of dapagliflozin including 5-bromo-2-chlorophenyl-2′-ethoxyldiphenylmethanone（1） and 5-bromo-2-chloro-2′-ethoxyl diphenylmethane（2） were synthesized. Impurity 1 was prepared via condensation, Fries rearrangement and ethylation using 5-bromo-2-chlorobenzoic acid and phenol as the starting materials. Impurity 2 was obtained from reduction of impurity 1.The structures of Impurity 1 and Impurity 2 were characterized using1 H NMR and MS.

关 键 词：达格列净 杂质 合成 

分 类 号：TQ333[化学工程—橡胶工业]