杂多酸催化7-羟基-4-甲基香豆素的无溶剂合成

Solvent-free synthesis of 7-hydroxy-4-methyl coumarin catalyzed by heteropolyacid

报道了以杂多酸(H3PW12O40、H3PMo12O40、H8SiW12O42、H6P2W18O40、H4SiW12O40、H6PMo6W6O40)为催化剂,以乙酰乙酸乙酯和间苯二酚为原料,通过Pechmann反应合成标题化合物的方法。探讨了以H4SiW12O40为催化剂时反应温度、催化剂用量、反应时间、原料比诸因素对产品收率的影响。实验表明,H4SiW12O40是合成标题化合物的良好催化剂,在反应温度为130℃,反应时间为50min,n(间苯二酚)∶n(乙酰乙酸乙酯)=1∶1.3,催化剂用量为1.5%(与间苯二酚的物质的量比)时,产品收率75.9%。

The synthesis of 7-hydroxy-4-methyl coumarin was catalyzed by different heteropolyaeids （ H3PW12O40, H3PMo12O40, H8SiW12O42 ,H6P2W18O40, H4SiW12O40 and H6PMo6W6O40） using ethylaeetoaeetato and resoreinol as the starting materials under solvent-free conditions. The optimum condition using H4SiW12O40 as the catalyst was as follows ： the molar ratio of ethylaeetoaeetato to resoreinol was 1.3 ： 1 ; the quantity of catalyst was equal to 1.5 % of resoreinol, the reaction temperature was 130℃, and the reaction time was 50 min. The yield of 7-hydroxy-4-methyl eoumarin could reach 75.9 %.