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以浓硫酸为催化剂 ,采用微波辐射技术 ,由间苯二酚与乙酰乙酸乙酯缩合制备 7-羟基 - 4-甲基香豆素。结果表明 ,微波辐射合成 7-羟基 - 4-甲基香豆素的最佳反应条件为 :间苯二酚 5 .5 g,乙酰乙酸乙酯 6 .8m l,浓硫酸 1.5 ml,微波功率 2 40 W,微波辐射时间 6 min,产率 84.1%。不采用微波辐射 ,反应时间大于 10 h,产率78%。红外光谱分析表明 ,7-羟基 - 4-甲基香豆素的特征峰与 7-羟基 - 4-甲基香豆素的各官能团的吸收峰吻合 ,测定 7-羟基 - 4-甲基香豆素的熔点为 189～ 192℃。
Using concentrated sulfuric acid as catalyst, 7-hydroxy-4-methylcoumarin was synthesized from condensation of resorcinol and ethyl acetoacetate by microwave irradiation. The results showed that the optimum reaction conditions for the synthesis of 7-hydroxy-4-methylcoumarin under microwave irradiation were as follows: resorcinol 5.5 g, ethyl acetoacetate 6 .8 ml, concentrated sulfuric acid 1.5 ml, microwave power 2 40 W, microwave irradiation time 6 min, yield 84.1%. Without microwave irradiation, the reaction time is more than 10 h and the yield is 78%. Infrared spectrum analysis showed that the characteristic peaks of 7-hydroxy-4-methylcoumarin coincided with the absorption peaks of various functional groups of 7-hydroxy-4-methylcoumarin, and 7-hydroxy-4- The melting point of 189 ~ 192 ℃.