【摘要】 以4-甲基-2-氨基吡啶为原料,利用相转移催化法,经酰化、氧化和水解三步反应合成了异烟肼(又称雷米封)衍生物的重要中间体2-氨基异烟酸。较佳的合成工艺条件是:酰化反应,以5g 4-甲基-2-氨基吡啶,4.36g乙酰氯为原料,4.17g冰醋酸为溶剂,在110℃下回流12h,得4-甲基-2-乙酰氨基吡啶粗产物5.96g,粗产率为85.8%;氧化和水解反应,以15g 4-甲基-2-乙酰氨基吡啶为原料,39g高锰酸钾、0.92g(3%)CTAC进行催化氧化,60℃下反应5h,得2-乙酰氨基-4-吡啶甲酸;再以此为原料碱水解,得2-氨基异烟酸12.07g,粗产率为87.5%。产物结构通过熔点分析和红外光谱进行表征。更多还原

【Abstract】 2-Aminoisonicotinic acid,an important intermediate of isoniazid derivatives,was synthesized from 4-methyl-2-aminopyridine by acylation,oxidation and hydrolysis with phase transfer catalysis.The optimum reaction conditions are obtained.The crude product of 4-methyl-2-acetylamino-pyridine was 5.96 g and the crude yield was 85.8% when 4-methyl-2-pyridine of 5g and acetyl chloride of4.36 g were used as raw materials,glacial acetic acid of 4.17 g was used as solvent and refluxed 12 h at 110 ℃ in acylation reaction.2-Acetylamino-4-pyridine carboxylic acid was got from 4-methyl-2-acetylamino-pyridine of 15 g,potassium permanganate of 39 g and the CTAC of 0.92g(3%)under catalytic oxidation by reacting for 5hat 60℃in oxidation and hydrolysis reaction.It was then used as raw material for base hydrolysis to got 2-aminoisonicotinic acid of 12.07 g and crude yield of 87.5%.The product structures were characterized by melting point analysis and IR spectroscopy.更多还原