摘要
研究了以胡椒环为原料,首先与乙醛酸反应,得中间体3,4-亚甲二氧基苯乙醇酸,然后以硝酸银对该中间体进行氧化脱羧,最后得到洋茉莉醛。并对第二步反应中的硝酸银用量、过硫酸钠的用量和反应温度等条件对收率的影响进行了研究。实验结果表明第二步反应的适宜条件为:反应温度为60℃、反应时间8 h、n(AgNO3)/n(3,4-二氧亚甲基苯乙醇酸)=0.008、n(Na2S2O8)/n(3,4-二氧亚甲基苯乙醇酸)=1.2;最终收率为75.9%。
Heliotropin was synthesized by reacting AgNO3 with 3,4-dioxymethylene mandelic acid, which was prepared from 1,3-benzodioxole. The effect of the amount of AgNO3 and Na2S2O8 and temperature on yield was investigated. The suitable conditions of synthesis were as follows reaction temperature was 60℃, reaction time was 8 h, n （AgNO3）/n （3,4-dioxymethylene mandelic acid） = 0. 008, and n （ Na2S2O8 ）/n （3,4-dioxymethylene mandelic acid）= 1.2. The overall yield was 75.9%.
出处
《化学世界》
CAS
CSCD
北大核心
2008年第3期164-165,177,共3页
Chemical World
关键词
洋茉莉醛
胡椒环
硝酸银
heliotropin
1,3-benzodioxole
silver nitrate
