第 40 卷第 3 期 |  | Vol. 40 No. 3 | 2010 年 6 月 | Jun 2010 |
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所屬欄目:醫藥及中間體
4-甲氧基二苯甲酰甲烷合成新方法研究 |
李敏誼1,魏 丹2,董 剛1,林序吟1,周 銳1
(1.廣東藥學(xué)院 藥科學(xué)院,廣東 廣州 510006;2.中山市食品藥品監督管理局 廣東 中山 528437) |
摘 要:研究了微波輻射合成4-甲氧基二苯甲酰甲烷。得到優(yōu)化合成條件為:n(對甲氧基苯乙酮) ∶ n(苯甲酸乙酯) ∶ n(氨基鈉)=1 ∶ 15 ∶ 4,微波輻射功率320 W,反應時(shí)間為45 min,與傳統加熱法相比,反應時(shí)間從7 h減少到45 min,收率從61.4%增加到77.4%。其結構經(jīng)元素分析、IR和1H NMR確證。 |
關(guān)鍵詞:4-甲氧基二苯甲酰甲烷;微波輻射;對甲氧基苯乙酮;苯甲酸乙酯 |
中圖分類(lèi)號:O625.4 文獻標識碼:A 文章編號:1009-9212(2010)03-0037-03 |
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Synthesis of 4-Methoxy-dibenzoyl methane with Microwave Irradiation |
LI Min-yi1,WEI Dan2,DONG Gang1,LIN Xu-yin1,ZHOU Rui1
(1. Department of Pharmacy,Guangdong Pharmaceutical University,Guangzhou 510006,China;2. The Food and Drug Administration of Zhongshan,Zhongshan 528437,China) |
Abstract:Microwave irradiation was used for the preparation of 4-methoxy-dibenzoyl methane from p-methoxy acetophenone and benzoate. The optimum conditions were found as follows:the molar ratio of p-methoxy acetophenone, ethyl benzoate and NaNH2 was 1 ∶ 15 ∶ 4, the power of microwave irradiation was 320 W and the reaction time was 45 min. The yield of the target compound was 77.4%. In comparison, the traditional method gives only 61.4% yield in much longer reaction time of 7 h. The product structure was confirmed by means of elemental analysis, IR and 1H NMR. |
Key words:4-methoxy-dibenzoylmethane;microwave irradiation;p-methoxy acetophenone; ethyl benzoate |
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作者簡(jiǎn)介:李敏誼(1955-),女,副教授,碩士生導師,主要從事有機藥物及精細化學(xué)品的合成研究。(E-mail:liminyigz@yahoo.com.cn)
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收稿日期:2010-05-10
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