摘要
以水杨醛与丙二酸二乙酯为原料制备香豆素-3-羧酸,利用其羧基与不同碳数的二溴烷烃反应得到相应的香豆素-3-羧酸溴代烷基酯,再与硝酸银反应生成香豆素-3-羧酸-硝氧烷基酯。目标化合物的结构经过红外光谱、核磁共振氢谱和质谱确证。考察了目标化合物合成中温度及投料比对反应的影响,得到最佳反应条件为:反应温度60℃,反应物配比竹(香豆素-3-羧酸溴代烷基酯):”(硝酸银)-1:3,此条件下目标化合物收率可达55.3%~90.8%。
Salicylaldehyde was reacted with diethyl malonate to give the raw material coumarin -3-carboxylic acid, which was then treated with dibromoalkanes to form brominated compounds. The brominated compounds reacted with silver nitrate to yield the target compounds. The chemical structure was confirmed by IR, MS and 1 H NMR spectroscopy. The effect of ratio of reagents and reaction temperature on the yield of the target compounds was studied. The optimum reaction conditions were as follows: n(intermediate):n(silver nitrate)= 1:3, and reaction temperature was 60℃. The yields of the target compounds were 55. 3%-90. 8%.
出处
《化学世界》
CAS
CSCD
2016年第7期420-423,共4页
Chemical World
基金
安徽省教育厅自然科学重点科研项目(KJ2013A168)