3,4-亚甲二氧基苯酚的化学合成

以胡椒胺为起始原料 ,在较温和的条件下 ,经重氮化、水解两步反应合成了目标产物 3 ,4亚甲二氧基苯酚。对水解工艺的研究表明 ,采用两相的水解萃取体系较好。以二氯甲烷为有机相 ,水油相的体积比为 1∶2 .4 ,滴加重氮盐时间为 4 h,水相中硫酸质量分数为 2 0 % ,在该条件下产率 80 % ,产品为淡黄色 ,纯度99.4 8%

SYNTHESIS OF 3,4-METHYLENEDIOXYPHENOL

Using 3,4(methylenedioxy)aniline as raw material, 3,4methylenedioxyphenol was synthesised in high yield under mild conditions through two steps of reaction, such as diazotization and hydrolysis. The hydrolysis step were recommended to adoptan an aq.organic twophases system in order to execute hydrolysis in aq. phase and extraction of product into organic phase simultaneousyl. Dichloromethane was used as the extracting agent. The hydrolysis conditions were as follow, the volume ratio of water phase to oil phase=1∶2.4; the time of dropping diazo salt 4 h; the mass fraction of sulfuric acid in the aq. phase 20%. Under these conditions, the yield reached 80%, and the color of the product was light yellow, purity 99.48%.