精细石油化工
精細石油化工
정세석유화공
SPECIALITY PETROCHEMICALS
2009年
5期
39-42
,共4页
糠醛丙二酸%α-呋喃丙烯酸%碱性离子液体%Knoevenagel反应
糠醛丙二痠%α-呋喃丙烯痠%堿性離子液體%Knoevenagel反應
강철병이산%α-부남병희산%감성리자액체%Knoevenagel반응
furfural%malonic acid%α-furylacrylic acid%basic ionic liquid%Knoevenagel reaction
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.
實驗以糠醛和丙二痠為原料,採用Knoevenagel法,以堿性離子液體為催化劑和溶劑,高效率閤成α-呋喃丙烯痠.討論瞭糠醛與丙二痠的用量、反應時間和溫度等對縮閤反應的影響.實驗結果錶明,最佳反應條件為:n([bmim]_2CO_3); n(糠醛); n(丙二痠)=1.3:1:1,反應溫度30℃,反應時間20 min,收率大于98%.產物後處理簡單,離子液體可多次循環使用.經覈磁共振、紅外光譜、質譜和元素分析對產物的結構進行瞭錶徵.
실험이강철화병이산위원료,채용Knoevenagel법,이감성리자액체위최화제화용제,고효솔합성α-부남병희산.토론료강철여병이산적용량、반응시간화온도등대축합반응적영향.실험결과표명,최가반응조건위:n([bmim]_2CO_3); n(강철); n(병이산)=1.3:1:1,반응온도30℃,반응시간20 min,수솔대우98%.산물후처리간단,리자액체가다차순배사용.경핵자공진、홍외광보、질보화원소분석대산물적결구진행료표정.
Basic ionic liquids,1-methyl-3-butyl imidazolium acetate [bmim]OAc,1-methyl-3-butyl imidazolium carbonate[bmim]_2CO_3 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 Ebmim]_2 CO_3 was the best catalyst and solvent in the synthesis of α-furylacrylic acid.The optimum reaction conditions are;n([bmim]_2 CO_3):n(furfural):n(malonic acid)=1.3:1:1,reaction temperature 30℃ and reaction time 20 min.Yield of α-furylacrylie 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.
