西他沙星关键手性中间体5-苄基-7-氨基-5-氮杂螺[2.4]庚烷的动力学拆分新方法  

A New Method for Kinetic Resolution of 5-Benzyl-7-amino-5-azaspiro[2.4]heptane,A Key Chiral Intermediate of Sitafloxacin

作　　者：汤朝哲 田芳[2] 王立新[2] TANG Chaozhe;TIAN Fang;WANG Lixin(University of Chinese Academy of Sciences, Beijing 100039, China;Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041, China)

机构地区：[1]中国科学院大学,北京100039 [2]中国科学院成都有机化学研究所,四川成都610041

出　　处：《合成化学》2022年第4期315-319,共5页Chinese Journal of Synthetic Chemistry

摘　　要：研究了西他沙星关键手性中间体5-苄基-7-氨基-5-氮杂螺[2.4]庚烷的手性拆分方法,分别研究了热力学拆分和动力学拆分对于不同构型的产物的区分。热力学拆分和动力学拆分均以较高的收率,得到99%对映选择性的产物。并对拆分剂,溶剂,温度,反应时间等影响因素进行了筛选。最终通过动力学拆分,降低了拆分剂的用量,降低了成本,有望实现工业化放大。A key chiral intermediate of Sitafloxacin,5-benzyl-7-amino-5-azaspiro[2.4]heptane is synthesized by the thermodynamic resolution and kinetic resolution.The influencing factors such as resolving agent,solvent,temperature and reaction time were screened.The dosage of the splitting agent is reduced,the cost is reduced,and industrial scale-up is realized.

关 键 词：西他沙星 手性胺 动力学拆分 热力学拆分 重结晶 

分 类 号：O62[理学—有机化学] R914.5[理学—化学]