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由乙酸酐和H2O2在无硫酸存在下合成过氧乙酸,然后向其滴加1,5-二萘酚的甲醇溶液,在一锅内简便地合成了胡桃醌。产物用苯重结晶,其结构经HPLC、UV-Vis、FTIR、1H NMR和13C NMR测试技术进行了表征和证实。考察了原料摩尔比、反应温度和反应时间对产率的影响。最佳反应条件为:n(1,5-二萘酚)∶n(乙酸酐)∶n(H2O2)=1∶4∶8,反应温度为40~60℃,反应时间为5.5 h,产率68%。结果表明,一锅法合成不用硫酸,无需真空蒸馏纯化过氧乙酸,是合成胡桃醌的简便方法。
Peroxyacetic acid was synthesized from acetic anhydride and H2O2 in the absence of sulfuric acid, and then a methanol solution of 1,5-naphthol was added dropwise thereto to easily synthesize juglone in one pot. The product was recrystallized from benzene and its structure was characterized and confirmed by HPLC, UV-Vis, FTIR, 1H NMR and 13C NMR techniques. The effects of molar ratio of raw materials, reaction temperature and reaction time on the yield were investigated. The optimal reaction conditions were: n (1,5-dinaphthol): n (acetic anhydride): n (H2O2) = 1: 4: 8, reaction temperature 40-60 ℃, reaction time 5.5 h, 68%. The results showed that the one-pot synthesis without sulfuric acid, without vacuum distillation purification of peracetic acid, is a simple method for the synthesis of juglone.