阿魏酸异辛酯的一锅法合成

One-pot Synthesis of 2-ethylhexyl-3-(4-hydroxy-3-methoxyphenyl)acrylate

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：香兰素用量6.08 g（0.04 mol），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，反应时间为8 h。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的目标产物进行了表征。

Abstract:

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 amion acid in isooctanol. We study the factors such as ratio of feed, and the amount of glycin and reaction time on product yeild. 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 8h, the yield of 2-ethylhexyl-3-(4-hydroxy-3- methoxyphenyl)acrylate was 75.2%. Its structure was characterized by 1HNMR and IR.