微波辐射四氯化锡催化无溶剂合成7-羟基-4-甲基香豆素

Synthesis of 7-hydroxy-4-methyl coumarin with microwave irradiation solvent-free catalyzed by SnCl_4·5H_2O

以间苯二酚和乙酰乙酸乙酯为原料,以五水四氯化锡为催化剂,采用微波辐射技术,无溶剂合成7-羟基-4-甲基香豆素。探索了不同反应条件对产率的影响。结果表明:当n(间苯二酚)∶n(乙酰乙酸乙酯)为1∶0.8,反应温度为115℃,五水四氯化锡为2.6 g(间苯二酚为0.15 mol),辐射时间为16 min,辐射功率为500 W时,产率可达80.6%。

The 1,3-benzenediol and ethyl acetoacetate as raw materials were used to synthesize 7-hydroxy- 4-methyl coumarin under microwave irradiation solvent-free with SnCl4· 5H2O as the catalyst. The effect of various reaction conditions on yield was explored, experimental results showed that：when the reaction con- ditions were as follow： n （1,3-benzenediol） ： n （ ethyl acetoacetate ） 1 ： 0.8, the reaction temperature 115 ℃, SnCl4 · 5 H2O 2.6 g （ 1,3-benzenediol 0.15 mol ）, the reaction time 16 rain, microwave radiation power 500 W,the yield reached up to 80.6%.