以2,6-二氯吡啶为起始原料,经甲氧基化、硝化、氨基化、还原及成环5步反应得到2-巯基-5-甲氧基咪唑并[4,5-b]吡啶,总收率45.7%. 重点比较了2-氯-6-甲氧基吡啶和2,6-二氯吡啶硝化反应条件及收率的差异,讨论了水合肼、NaOH的用量对目标产物收率的影响. 用1H NMR、MS和IR测试技术对目标产物结构进行了表征.
2-Mercapto-5-methoxyimidazo[4,5-b]pyridine was obtained with 2,6-dichloropyridine as the starting material in five steps, including methoxylation, nitration, amination, reduction and cyclization. The overall yield of 2-mercapto-5-methoxyimidazo[4,5-b]pyridine was up to 45.7%. The differences between reaction conditions and yields of nitration of 2-chloro-6-methoxypyridine and 2,6-dichloropyridine were discussed, the effects of the amounts of hydrazine hydrate and the amounts of sodium hydroxide on the yield of the target product were also discussed. The structure of the target product was identified by ~1H NMR, MS and IR.
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