摘要
实验以糠醛和丙二酸为原料,采用Knoevenagel法,以碱性离子液体为催化剂和溶剂,高效率合成α-呋喃丙烯酸。讨论了糠醛与丙二酸的用量、反应时间和温度等对缩合反应的影响。实验结果表明,最佳反应条件为:n([bmim]_2CO_3):n(糠醛):n(丙二酸)=1.3:1:1,反应温度30℃,反应时间20 min,收率大于98%。产物后处理简单,离子液体可多次循环使用。经核磁共振、红外光谱、质谱和元素分析对产物的结构进行了表征。
Basic ionic liquids, 1-methyl-3-butyl imidazolium acetate [-bmim]OAc, 1-methyl-3-butyl imidazolium carbonate [-bmim]2CO3 and 1-methyl-3-butyl imidazolium benzoate [bmim]PhCOO were prepared and used to catalyze the Knoevenagel condensation of furfural with malonic acid. The results show that the basic ionic liquid [-bmim]2CO3 was the best catalyst and solvent in the synthesis of α-furylacrylic acid. The optimum reaction conditions are. n （[bmim]2CO3） ： n （furfural） ： n （malonie acid） =1.3 ：1：1, reaction temperature 30 ℃ and reaction time 20 min. Yield of α-furylacrylic acid reaches 98%. The product could be conveniently separated, and the remaining basic ionic liquid could be reused for at least five times without much lose in activities. The product structure was characterized by 1H NMR, IR,MS spectra and elemental analysis.
出处
《精细石油化工》
CAS
CSCD
北大核心
2009年第5期39-42,共4页
Speciality Petrochemicals
