丙烯醛二乙缩醛温和液相反应制备3-甲基吡啶

Preparation of 3-Picoline by Mild Liquid Phase Reaction of Acrolein Diethyl Acetal

以丙烯醛二乙缩醛为原料,通过单因素实验建立了优化的温和液相反应条件。合成3-甲基吡啶的优化工艺条件为:以乙酸为溶剂,反应温度130℃,料比n(丙烯醛二乙缩醛)∶n(乙酸铵)∶n(乙酸)=1∶9.48∶21.33。溶剂为酸性,可以极大地促进反应的正向进行,起到了催化剂的作用。在优化条件下,实现了丙烯醛二乙缩醛转化率100%,3-甲基吡啶收率65.90%。

The synthesis of 3-picoline by mild liquid phase reaction using acolein diethyl acetal as raw material. The reaction conditions were optimized and the obtained opti- mum conditions were using acetic acid as solvent, temperature 130℃, n（acolein diethyl acetal） ： n（acetic ammonium） ： n（acetic acid）=1： 9.48 ： 21.33. Under above condi- tions, the conversion of acolein diethyl acetal was almost 100% and the yield of 3-pico- line was 65.90%.