微波辐射下磺酸基功能化离子液体无溶剂催化合成4-甲基香豆素及其衍生物

Synthesis of Coumarin Derivatives with Microwave Irradiation Solvent-Free Catalyzed by SO3H Functionalized Ionic Liquid

摘要:

研究了3种磺酸基功能化离子液体催化香豆素及其衍生物的合成，取代酚与乙酰乙酸乙酯在无溶剂微波辐射条件下，通过Pechmann缩合反应，合成了一系列4-甲基香豆素衍生物，探讨了反应时间、反应温度、催化剂用量、离子液体重复使用性能诸因素对产品收率的影响。结果表明，离子液体[C3SO3Hmim]HSO4是合成目标产物的良好催化剂，微波辐射时间10min，反应温度100℃，n(酚):n(乙酰乙酸乙酯)=1:1，催化剂用量x ([C3SO3Hmim]HSO4)=20%时，最高产率可达94％。该方法反应条件温和，操作简便，产物易分离，产率高，环境友好，离子液体可重复使用4次。

Abstract:

The coumarin derivatives of phenols and ethyl acetoaceate were carried out using SO3H functionalized ionic liquid as the catalysts via Pechmann condensation. The optimum reaction condition: n(phenols):n(ethyl acetoaceate)=1:1, microwave irradiation reaction time 10 minute and reaction temperature 100℃. The high yield can reach 94％ in the presence of x([C3SO3Hmim]HSO4)=20% as catalyst, under solvent-free conditions. This method has the advantages of mild reaction conditions, easy operation, high yields and environmental begin. Moreover, the catalyst could be reused for at least four times.