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[目的]2,3-二氯-5-甲基吡啶是一类重要的精细化工中间体,开发出一种合成2,3-二氯-5-甲基吡啶的新方法,并优化其合成工艺。[方法]以5-甲基-3,4-二氢吡啶-2(1H)-酮和氯气为起始原料,在三氯化铁及N,N,N’,N’,N’’-五甲基二亚乙基三胺(PMDETA)的催化下合成2,3-二氯-5-甲基吡啶。考察催化剂、配体、温度等因素对反应的影响。[结果]在优化的反应条件下,2,3-二氯-5-甲基吡啶收率75%,纯度99.5%。[结论]该方法操作简单安全,三废少,适合工业化生产。
[Objective] As an important class of fine chemical intermediates, 2,3-dichloro-5-methylpyridine was developed as a new method for the synthesis of 2,3-dichloro-5-methylpyridine and its synthesis was optimized Process. [Method] With 5 - methyl - 3,4 - dihydropyridin - 2 (1H) - one and chlorine as the starting materials, ferric chloride and N, N, N ’, N’, N " Synthesis of 2,3-dichloro-5-methylpyridine catalyzed by pentamethyldiethylenetriamine (PMDETA). Investigate the catalyst, ligand, temperature and other factors on the reaction. [Result] Under the optimized reaction conditions, the yield of 2,3-dichloro-5-methylpyridine was 75% and the purity was 99.5%. [Conclusion] The method is simple and safe to operate, less waste and suitable for industrial production.