| 引用本文： |
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丁国华,刘峥,沈方明.微波辐射合成7-羟基-4-甲基香豆素[J].广西科学,2002,9(1):46-47,52. [点击复制]
- Ding Guohua,Liu Zheng,Shen Fangmin.Synthesis of 7-Hydroxy-4-Methylcoumarin under Microwave Irradiation[J].Guangxi Sciences,2002,9(1):46-47,52. [点击复制]
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| 摘要: |
| 以浓硫酸为催化剂,采用微波辐射技术,由间苯二酚与乙酰乙酸乙酯缩合制备7-羟基-4-甲基香豆素。结果表明,微波辐射合成7-羟基-4-甲基香豆素的最佳反应条件为:间苯二酚5.5g,乙酰乙酸乙酯6.8ml,浓硫酸1.5ml,微波功率240W,微波辐射时间6min,产率84.1%。不采用微波辐射,反应时间大于10h,产率78%。红外光谱分析表明,7-羟基-4-甲基香豆素的特征峰与7-羟基-4-甲基香豆素的各官能团的吸收峰吻合,测定7-羟基-4-甲基香豆素的熔点为189~192℃。 |
| 关键词: 7-羟基-4-甲基香豆素 微波辐射 间苯二酚 乙酰乙酸乙酯 |
| DOI： |
| 投稿时间：2001-07-12修订日期：2001-11-22 |
| 基金项目: |
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| Synthesis of 7-Hydroxy-4-Methylcoumarin under Microwave Irradiation |
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Ding Guohua, Liu Zheng, Shen Fangmin
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| (Dept. of Material and Chemical Engin, Guilin Institute of Technology, 12 Jianganlu, Guilin, Guangxi, 541004, China) |
| Abstract: |
| The synthesis of 7-hydroxy 4-methylcoumarin is performed by the condensation of 1,3-benzenediol and ethyl acetoacetate under microwave irradiation. The optimum reaction conditions are as follows:5.5 g 1,3-benzenedol,6.8 ml ethyl acetoacetate,1.5 ml concentrated sulfuric acid, 240 W microwave power and 6 min microwave irradiation. The yield reachs 84.1%. In the non irradiated conditions, the yield is 78%,and the reaction time is over 10 h.IR spectra indicates that the characteristic peaks of 7-hydroxy 4-methylcoumarin are in line with the absorption peaks of other functional groups. The melting point of 7-hydroxy 4-methylcoumarin is 189℃ to 192℃. |
| Key words: 7-hydroxy 4-methylcoumarin microwave irradiation 1,3-benzenediol ethyl acetoacetate |
