摘要
合成了西他沙星及其有关物质D-2,总收率78.7%。并对其进行了MS、HNMR和TG等表征;研究了氢化脱苄的反应条件、缩合反应的后处理优化和脱Boc的盐酸用量,优化的条件为:脱苄反应10%钯炭,回流反应0.5 h,缩合反应后处理溶剂比例v(乙腈)∶v(水)=1∶2,脱Boc的盐酸用量为15 mol倍量。
Sitafloxacin and its related substance D-2 were obtained with a total product yield of 78.7%. The structures of Sitafloxacin and intermediates from the step reactions were confirmed using MS, HNMR and TG. The optimal conditions for each step reaction were as following： in the debenzylation reaction,10% of Pd/C with a reflux time of 0.5 h was adopted; in the post-treatment of condensation reaction, a mixed solvent of water and acetonitrile with a volume ratio of 2：1 was used; in the deprotection of N-boc reaction, the amount of hydrochloric acid was 15 times of the substrate in mole.
出处
《精细化工中间体》
CAS
2015年第5期30-33,共4页
Fine Chemical Intermediates
基金
苏州市科技发展计划项目(ZXY2012004)
关键词
西他沙星
D-2
氢化
脱苄
sitafloxacin
D-2
hydrogenation
debenzylation
