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陈海涛, 马攀龙, 杨柳, 韩福娇, 王文新, 杨振强. 6-溴-3-氟-2-甲氧基吡啶的合成及工艺[J]. 信阳师范学院学报(自然科学版), 2020, 33(1): 102-105. DOI: 10.3969/j.issn.1003-0972.2020.01.017
引用本文: 陈海涛, 马攀龙, 杨柳, 韩福娇, 王文新, 杨振强. 6-溴-3-氟-2-甲氧基吡啶的合成及工艺[J]. 信阳师范学院学报(自然科学版), 2020, 33(1): 102-105. DOI: 10.3969/j.issn.1003-0972.2020.01.017
shu
CHEN Haitao, MA Panlong, YANG Liu, HAN Fujiao, WANG Wenxin, YANG Zhenqiang. Synthesis and Preparation Process of 6-bromo-3-fluoro-2-methoxypyridine[J]. Journal of Xinyang Normal University (Natural Science Edition), 2020, 33(1): 102-105. DOI: 10.3969/j.issn.1003-0972.2020.01.017
Citation: CHEN Haitao, MA Panlong, YANG Liu, HAN Fujiao, WANG Wenxin, YANG Zhenqiang. Synthesis and Preparation Process of 6-bromo-3-fluoro-2-methoxypyridine[J]. Journal of Xinyang Normal University (Natural Science Edition), 2020, 33(1): 102-105. DOI: 10.3969/j.issn.1003-0972.2020.01.017
shu

6-溴-3-氟-2-甲氧基吡啶的合成及工艺

Synthesis and Preparation Process of 6-bromo-3-fluoro-2-methoxypyridine

    摘要
  • 摘要: 以3-氨基吡啶为原料，通过溴化、亲核取代反应合成中间体6-溴-2-甲氧基-3-氨基吡啶，最后经重氮化反应合成了目标产物6-溴-3-氟-2-甲氧基吡啶，产物结构经过了核磁、液质表征.研究了溴化工艺、溶剂以及甲醇钠对产物收率的影响.结果表明：采用的路线溴化反应后处理无需柱层析或重结晶，收率高；第二步反应优化了溶剂，收率提高到90.1%.

     

    Abstract: 6-bromo-2-methoxyl-3-aminopyridine is synthesized with 3-aminopyridine through bromination reaction and nucleophilic substitution, and then is performed a diazotization reaction process to obtain 6-bromo-3-fluoro-2-methoxypyridine. The product is characterized by NMR and LC-MS. The effects of bromination processes, solvent and sodium methanol on the yield are studied.The results show that this method does not require column chromatography or recrystallization, and the yield is high. The solvent is optimized in the second step and the yield increases to 90.1%.

     

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