3-甲氨基吡啶的合成研究

• 作 者: 穆飞虎 戴本林 徐宁 朱安峰
• 机 构: 淮阴师范学院化学化工学院,
• 出 处: 化学工程与装备
• 发表日期: 2016年12期
• 关键词: 甲氨基 甲酰化 3-甲氨基吡啶 3-氨基吡啶 最佳条件 室温反应 还原条件 高效液相色谱 乙酸酐 硼氢化钠还原

以3-氨基吡啶为原料,经两步反应合成得到3-甲氨基吡啶,同时对合成条件进行了优化。研究结果表明,最优甲酰化条件为:将甲酸滴加至乙酸酐中在55℃反应2h,然后降至20℃加入3-氨基吡啶,反应15min;最佳还原条件为:n(Li Al H4)∶n(3-甲酰氨基吡啶)=1.6,室温反应2h。在最佳条件下,3-甲氨基吡啶的收率为88.4%。通过高效液相色谱分析产品,并利用核磁共振氢谱鉴定产品。

3-aminopyridine was used as the starting material to synthesize 3-methylaminopyridine by two steps. The synthesis conditions were also optimized. The results showed that the optimal conditions for formylation were as follows: formic acid was added dropwise to acetic anhydride for 2h at 55 ° C, then 3-aminopyridine was added to reduce the temperature to 20 ° C and reacted for 15min. The optimum reduction conditions were as follows: Li H4): n (3-formamidopyridine) = 1.6, and reacted at room temperature for 2h. Under the optimal conditions, the yield of 3-methylaminopyridine was 88.4%. The product was analyzed by high performance liquid chromatography, and the product was identified by 1H nuclear magnetic resonance spectroscopy.