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以2-甲氧基吡啶为起始原料,首先采用二异丙胺生成LDA,再与正丁基锂合成有机锂试剂,然后硼基化,水解共四步反应得到2-甲氧基-3-吡啶硼酸。考察了各步反应的物料比,反应温度,反应时间的影响。结果:生成2-甲氧基-3-吡啶锂试剂时2-甲氧基吡啶的用量为6g,反应时间为1h,反应温度为-45℃;生成2-甲氧基-3-吡啶硼酸酯时硼酸三丁酯的用量为17.5g,反应时间为1h,反应温度为-45℃。最终产率为63.3%。
Starting from 2-methoxypyridine, LDA was firstly synthesized from diisopropylamine and then organolithium reagent was synthesized from n-butyllithium, and then borated and hydrolyzed to obtain 2-methoxy-3- Pyridine boronic acid. The effects of material ratio, reaction temperature and reaction time on the reaction were investigated. Results: The amount of 2-methoxypyridine was 6g, the reaction time was 1h and the reaction temperature was -45 ℃. The yield of 2-methoxy-3-pyridyl boronic acid The amount of tributyl borate was 17.5g, the reaction time was 1h and the reaction temperature was -45 ℃. The final yield was 63.3%.