摘要
以4-甲基-3-溴吡啶为起始原料，在甲基叔丁基醚中先和正丁基锂发生溴锂交换然后和硼酸三异丙酯反应，用3N盐酸淬灭后得到了4-甲基-3-吡啶硼酸。在该反应中考察了反应溶剂、加料顺序和溶剂体积对反应的影响。使用HPLC，LCMS，^1HNMR等方法对反应终点及产品结构进行分析和表征。通过实验得出较优的工艺条件，以150g4-甲基-3-溴吡啶为起始原料来验证工艺，反应收率为69．9％，纯度为98．7％。
3-bromo-4-methylpyridine, n-butyllithium and isopropyl borate were used as starting material to prepare 4-menthyl-3-pyridylhoronic acid. In the reaction, bromine lithium exchange was occurred firstly between 3-bromo-4-methylpyridine and n-butyl lithium, then reacted with isopropyl borate, and then queenched with 3N HC1. The effect of reaction solvent, addition sequence and volume of solvent were investigated. Purity, structure of the product and in process control were characterized by HPLC, LCMS and H NMR. The optimized process conditions were obtained, and the optimized process conditions were evaluated on 150 g scale, the yield was 69.9% and the purity was 98.7%.
基金
安徽省科技攻关计划项目（1501ZC03030）,亳州师范高等专科学校校级科研课题（BSKY201432）
