微波辐射碳酸钾催化无溶剂合成3-取代苯并香豆素  

Solvent-Free Synthesis of 3-Substituted Benzocoumarin Catalyzed by K_2CO_3 under Microwave Irradiation

作　　者：曾育才[1] 李岚[1] 梁奇峰[1] 刘小玲[1] 

机构地区：[1]嘉应学院化学与环境学院,广东梅州514015

出　　处：《嘉应学院学报》2013年第11期40-44,共5页Journal of Jiaying University

基　　金：梅州市科技局与嘉应学院资助项目(2012KJZ03)

摘　　要：在微波辐射和无溶剂条件下,以2-羟基萘甲醛和乙酰乙酸乙酯或丙二酸二乙酯为原料,利用环境友好的K2CO3作催化剂,通过Knoevenagel缩合反应快速简便的合成了2种3-取代苯并香豆素(3).通过正交试验获得优化工艺条件为:2-羟基-1-萘甲醛用量20mmol,乙酰乙酸乙酯或丙二酸二乙酯40mmol,无水碳酸钾用量0.0552g,微波功率300W、温度100℃,无溶剂条件下微波反应3min,平均收率可达82.2%(3a)或85.7%(3b).K2CO3 was utilized as an friendly catalyst for the environmentally fast and simple synthesis of two 3-sub- stituted benzocoumarin（ 3） by the Knoevenagel condensation of 2- hydroxy- 1- naphthaldehyde with ethyl aceto- aceate or diethyl malonate under microwave irradiation and solvent free conditions. The optimum parameters were obtained as： dosage of 2- hydroxy- 1- naphthaldehyde 20mmol,ethyl acetoaceate or diethyl malonate 40mmol, K2CO30. 0552g,power of microwave irradiation 300W,temperature of microwave 100℃,time of microwave 3min under solvent free conditions. Under this optimized condion,average yield of 3-acetyl benzocoumarin（ 3a） a- chieves 82. 2% and benzocoumarin- 3- ethyl formate（ 3b） 85. 7%.

关 键 词：KNOEVENAGEL缩合反应 3-取代苯并香豆素 2-羟基-1-萘甲醛 K 2 CO 3 无溶剂合成 

分 类 号：TQ655[化学工程—精细化工]