过氧化氢氧化糠胺制备3-羟基吡啶

PREPARATION OF 3-HYDROXYPYRIDINE FROM 2-AMINOMETHYLFURAN WITH HYDROGEN DIOXIDE AS OXIDANT

以糠胺为原料、H2O2为氧化剂制备3-羟基吡啶。考察了盐酸浓度、反应温度和反应时间对3-羟基吡啶收率的影响。最佳反应条件为:n(糠胺),n(盐酸):n(过氧化氢)=1．0:5．0:1．1,在0-5℃4 h内将过氧化氢滴加入糠胺和盐酸的混合物中,加热回流反应0．5 h,得目标产物,收率76％,质量分数99．3%。

3-hydroxypyridine was prepared by reacting furfurylamine with H2O2 in the presence of HCl, followed by hydrolysis. The optimal conditions were found as fellows, molar ratio of furfurylamine ： HCl ： H2O2=1 ： 5 ： 1.1, and H2O2 added dropwisely at 0 - 5 ℃, and then refluxed at 100 - 105 ℃ for 0.5 h. After working up, 3-hydroxypyridine was obtained in 76% yield and 99.3% purity. The effects of reaction temperature, time and the concentration of hydrochloric acid on the yield of 3-hydroxypyridine were investigated.