SO_4^(2-)/ZrO_2催化香料α-呋喃丙烯酸丁酯的合成

A simplified method for synthesis of aroma compound butyl α-furancrylate catalyzed by SO_^(2-4)/ZrO_2

采用SO42-/ZrO2作催化剂,在无溶剂条件下,糠醛经Knoevenagel缩合和酯化反应一锅法合成了香料α-呋喃丙烯酸丁酯。结果表明,在糠醛0.1 mol,丙二酸0.1 mol,催化剂0.96 g,反应80 min条件下,糠醛与丙二酸发生Knoevenagel缩合得到α-呋喃丙烯酸,糠醛转化率99.1%;产物不经分离直接与0.13 mol丁醇酯化反应2 h合成了α-呋喃丙烯酸丁酯,产率92.5%,产物具有焦糖样甜香并兼有微弱水果香气。催化剂重复使用8次后活性无显著降低。

A simplified method for synthesis of butyl α-furancrylate using furaldehyde,malonic acid and butanol as starting materials as well as SO4^2-/ZrO2 as catalyst was developed.The whole process consists of Knoevenagel condensation as the first step and followed by esterification.Accessory solvent and separation operation of the intermediate from the first step reaction mixture are not needed.Under conditions as 0.1 mol of furaldehyde with 0.1 mol of malonic acid and 0.96 g of the catalyst,reaction with reflux for time 80 min,the conversion of furaldehyde achieves 99.1%.The intermediate product mixture of the first step was further reacted with 0.13 mol of butanol for 2 h and the yield of butyl α-furancrylate achieves 92.5%.Flavor of the product displays sweet scent that similar to caramel with slight fruit odor.The catalyst can be reused for 8 times without significant decline of the activity.