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作 者:梅苏宁[1] 俞迪虎[1] 李勇[1] 徐超峰[1]
机构地区:[1]浙江大学化学工程与生物工程学系,浙江杭州310027
出 处:《化学研究》2010年第1期64-67,共4页Chemical Research
摘 要:以2-甲基吡啶为原料,水为溶剂,经80℃下高锰酸钾氧化和乙醇重结晶得到2-甲酸吡啶;采用红外光谱仪和核磁共振谱仪表征了目标产物的结构;考察了高锰酸钾用量、溶剂用量和反应时间对产物收率的影响,讨论了重结晶试剂的选择,进而确定了合成2-甲酸吡啶的较优条件.结果表明:以水作反应溶剂,控制原料和高锰酸钾的摩尔比为1:2.3时,反应时间为5~6h,以乙醇重结晶,目标产物的总收率达79.7%.2-Pyridinecarboxylic acid was synthesized by oxidizing 2-methylpyridine at 80℃ with potassium permanganate in the presence of water as the solvent and in connection with reerystallization in ethanol. The product was characterized by means of infrared spectrometry and nuclear magnetic resonance spectrometry. The effects of potassium permanganate amount, solvent amount and reaction time on yield of the product were investigated, while the selection of the solvents for recrystallization was discussed. Then the optimal conditions for synthesizing 2-pyridinecarboxylic acid were determined. Results indicate that by keeping the molar ratio of 2- methylpyridine to potassium permanganate in water as 1 : 2.3 and reaction time as 5-6 h, the target product recrystalized with ethanol can be obtained at an overall yield of 79.7%.
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