3-甲基吡啶的微波液相法合成

Liquid-phase Synthesis of 3-Picoline Under Microwave Irradiation

在液相条件下,采用微波协助合成3-甲基吡啶(1),其结构经GC-MS确证。研究了碳源(甘油、丙烯醛二甲缩醛和丙烯醛二乙缩醛)、氨源(硫酸亚铁铵、乙酸铵和氨水)、固体催化剂用量和溶剂(水、离子液体、二乙二醇甲醚、乙二醇丁醚和二甲基亚砜)对1合成反应的影响。结果表明:丙烯醛是重要的中间产物;在多相催化体系下,1收率最高可达到19.8%。

3-Picoline( 1) was synthesized by liquid-phase method under microwave irradiation. The structure was confirmed by GC-MS. Various influencing parameters,including carbon sources( glycerol,acrolein dimethyl acetal and acrolein diethyl acetal),ammonia sources( ammonium ferrous sulfate,ammonium acetate and ammonium hydroxide),amount of heterogeneous catalyst and solvent( water,ionic liquid,diethylene glycol monomethyl ether,ethylene glycol monobutyl ether and dimethyl sulfoxide) on the synthesis of 1 were investigated. The results indicated that acrolein was an important intermediate and the highest yield of 1 achieved 19. 8%.