摘要
目的:探讨医药中间体吡啶-2-硼酸的制备方法。方法:以异丙基氯化镁为格氏试剂,2-溴吡啶和硼酸三(三甲硅烷基)酯为原料,在氮气保护下,通过格氏反应合成目标产物,用核磁共振确认产物结构。结果:合成了吡啶-2-硼酸,确证了产物结构;优化反应条件为:物料比n(硼酸酯)∶n(2-溴吡啶)=2∶1,反应温度0℃,反应时间3 h,水解温度0℃,总收率达67.7%。结论:采用格氏反应制备吡啶-2-硼酸,反应条件温和,产物收率较高,有助于吡啶类药物的开发和研究。
Objective：To investigate the means of preparing 2-pyridylboronic acid.Methods：The product was synthesized with 2-bromopyridine,tris-trimethylsilylborate and iPrMgCl as Grignard reagents under N2,and identified by 1H-NMR.Results：2-pyridylboronic acid was synthesized with the yield of 67.7% on conditions of n（tris-trimethylsilylborate）∶n（2-bromopyridine）=2∶1;the reaction temperature was 0 ℃,the reaction time 3 hours and the hydrolysis temperature 0 ℃.Conclusions：2-pyridylboronic acid can be synthesized by Grignard reaction on moderate conditions with high yield,which may contribute to the study of pyridine drugs.
出处
《蚌埠医学院学报》
CAS
2010年第10期1043-1045,共3页
Journal of Bengbu Medical College
基金
蚌埠医学院科研资助项目(BY0743)
