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出 处:《精细化工》2010年第8期793-795,799,共4页Fine Chemicals
基 金:华侨大学校级科研基金(07HZR16)~~
摘 要:用香兰素、丙二酸二乙酯、异辛醇、冰醋酸为主要原料,以甘氨酸为催化剂,经Knoenenagel缩合反应,一锅法合成了阿魏酸异辛酯。研究了原料摩尔比、甘氨酸用量、反应时间等对阿魏酸异辛酯收率的影响。结果表明,最佳反应条件:香兰素6.08g(0.04mol),n(丙二酸二乙酯)/n(香兰素)=1.4,n(甘氨酸)/n(香兰素)=0.15,n(异辛醇)/n(丙二酸二乙酯)=12,反应时间8h,在该条件下目标产物阿魏酸异辛酯产率达75.2%。用核磁共振波谱及红外光谱对所得目标产物进行了表征。2-Ethylhexyl-3-(4-hydroxy-3-methoxyphenyl)acrylate was synthesized from 4-hydroxy-3-methoxybenzaldehyde and diethyl malonate by Knoevenagel condensation under the catalysis of amino acid in isooctanol.The factors such as the ratio of feed,the amount of glycin and reaction time on product yield were investigated.The best reaction condition:stating from 6.08 g(0.04 mol) 4-hydroxy-3-methoxybenzaldehyde,n(diethyl malonate)/n(4-hydroxy-3-methoxy-benzaldehyde)=1.4,n(glycin)/n(4-hydroxy-3-methoxybenzaldehyde)=0.15,n(isooctanol)/n(diethyl malonate)=12,and reacting for 8 h,the yield of 2-ethylhexyl-3-(4-hydroxy-3-methoxyphenyl)acrylate was 75.2%.Its structure was characterized by 1HNMR and IR.
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