达格列净中两种杂质的合成及表征  

Synthesis and Characterization of Two Impurities in Dapagliflozin

作　　者：杨学军 杜渭松 赵俊丰 高嫒嫒 别国军 YANG Xue-jun;DU Wei-song;ZHAO Jun-feng;GAO Ai-ai;BIE Guo-jun(Xi'an Caijing Opto-Electrical Science&Technology Co.,Ltd.,Xizan 710065,China)

机构地区：[1]西安彩晶光电科技股份有限公司,陕西西安710065

出　　处：《精细化工中间体》2020年第4期34-37,共4页Fine Chemical Intermediates

基　　金：陕西省科技计划(第二批)-技术创新引导计划(陕科发[2019]11号)。

摘　　要：以邻氯苯酚和2-氯-5-碘苯甲酸为主要原料,经乙基化、酰氯化、格氏偶联反应、还原反应,定向合成了降糖药达格列净中的两种相关邻位取代杂质2-氯-5-碘-2′-乙氧基二苯甲酮(4)和2-氯-5-碘-2′-乙氧基二苯甲烷(5),并对其进行了GC-MS、IR、NMR等结构确证。Two related ortho-substituted impurities,2-chloro-5-iodo-2’-ethoxybenzophenone(4)and 2-chloro-5-iodo-2’-ethoxydiphenylmethane(5),were synthesized from o-chlorophenol and 2-chloro-5-iodobenzoic acid through reactions including ethylation,acyl chlorination,Grignard coupling reaction and reduction reaction.The structures of the products were characterized by GC-MS,IR and NMR.

关 键 词：达格列净 邻位取代杂质 2-氯-5-碘-2′-乙氧基二苯甲酮 2-氯-5-碘-2′-乙氧基二苯甲烷 

分 类 号：O625.21[理学—有机化学]