无溶剂下微波辐射合成阿魏酸

Solvent-free synthesis of ferulic acid under microwave irradiation

以香草醛为反应底物,丙二酸为试剂,醋酸铵为催化剂,采用微波辐射技术,经Knoevenagel-Doebner反应,在无溶剂条件下合成了阿魏酸。研究了酸、醛和醋酸铵用量,微波功率和辐射时间对阿魏酸收率的影响。得到较佳工艺条件为:40 mmol香草醛、48 mmol丙二酸、4.8 mmol醋酸铵,微波功率400 W,辐射15 min。在此条件下产率为86.9%,阿魏酸的质量分数超过98%。

Ferulic acid was synthesized from vanillin and malonic acid by Knoevenagel - Doebner condensation with ammonium acetate as catalyst under microwave irradiation without solvent. Effects of molar ratio of vanillin to malonic acid, the dosage of ammonium acetate, microwave power and time of irradiation on the yield of ferulic acid were investigated. The optimum conditions for the synthesis of ferulic acid are： molar ratio of 40 mmol vanillin, 48 mmol malonic acid, 4. 8 mmol ammonium acetate, microwave power 400 W, time of irradiation 15 min. Under this optimum reaction conditions, the yield achieves 86. 9%, and the purity of ferulic acid achieves higher than 98%.