摘要
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5．5h，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。
5-Hydroxy-1,4-naphthoquinone was synthesized in one pot by dropping methanol solution of 1,5- dihydroxy naphthalene to peroxyacetic acid formed from acetic anhydride and hydrogen peroxide without H2SO4 with a yield of 68%. The product was purified by recrystallization from benzene, and its structure was confirmed by HPLC, UV, FTIR, ^1H NMR and ^13C NMR. The reaction conditions, such as the ratio of the reactants, reaction temperature and reaction time, were optimized. The optimum molar ratio was 1：4：8 of 1,5- dihydroxy naphthalene, acetic anhydride and hydrogen peroxide. The reaction temperature was 40-60 ℃ and the reaction time 5.5 h. The results suggest that the one-pot-method is an efficient and convenient synthesis approach of juglone without using H2SO4 and purification of peroxyacetic acid by vacuum distillation.
出处
《应用化学》
CAS
CSCD
北大核心
2007年第12期1470-1472,共3页
Chinese Journal of Applied Chemistry
关键词
胡桃醌
羟基萘醌
一锅法
合成
Juglone, hydroxy-naphthoquinones, one-pot-method, synthesis
