微波辐射碳酸钾催化无溶剂合成3-取代苯并香豆素 |
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引用本文: | 曾育才,李岚,梁奇峰,刘小玲.微波辐射碳酸钾催化无溶剂合成3-取代苯并香豆素[J].嘉应学院学报,2013(11):40-44. |
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作者姓名: | 曾育才 李岚 梁奇峰 刘小玲 |
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作者单位: | 嘉应学院化学与环境学院,广东梅州514015 |
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基金项目: | 梅州市科技局与嘉应学院资助项目(2012KJZ03) |
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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).
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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 |
Solvent-Free Synthesis of 3-Substituted Benzocoumarin Catalyzed by K_2CO_3 under Microwave Irradiation |
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Institution: | ZENG Yu -cai, LI Lan, LIANG Qi -feng , LIU Xiao -ling ( School of Chemistry and Environment, Jiaying University, Meizhou 514015, China) |
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Abstract: | 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%. |
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Keywords: | Knoevenagel condensation 3-substituted benzocoumarin 2-hydroxy-1-naphthaldehyde K2CO3 solvent-free synthesis |
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