第 39 卷第 2 期 |  | Vol. 39 No. 2 | 2009 年 4 月 | Apr 2009 |
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所屬欄目:醫藥及中間體
苯磺酸催化合成7-羥基-4-甲基香豆素 |
張芳芳,姜 恒*,宮 紅,程月紅
(遼寧石油化工大學(xué) 化學(xué)與材料科學(xué)學(xué)院,遼寧 撫順 113001) |
摘 要:以苯磺酸作催化劑,乙酰乙酸乙酯和間苯二酚為原料,通過(guò)Pechmann縮合反應合成7-羥基-4-甲基香豆素?疾炝嗽吓浔、催化劑用量和反應溫度對產(chǎn)品收率的影響,得到較適宜的合成條件為:在110℃下,催化劑用量為0.5%(以間苯二酚計,n/n),n(乙酰乙酸乙酯)∶n(間苯二酚)=1.3∶1時(shí),反應21 min,平行實(shí)驗的平均收率為85.0%。產(chǎn)品結構用IR表征。 |
關(guān)鍵詞:7-羥基-4-甲基香豆素;苯磺酸;Pechmann縮合反應;合成 |
中圖分類(lèi)號:TQ203.3 文獻標識碼:A 文章編號:1009-9212(2009)02- 0035-03 |
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Synthesis of 7-Hydroxy-4-methylcoumarin Using Phenyl Sulfonic Acid as Catalyst |
ZHANG Fang-fang,JIANG Heng*,GONG Hong,CHENG Yue-hong
(College of Chemistry and Materials Science,Liaoning Petrochemical University,Fushun 113001,China) |
Abstract:7-Hydroxy-4-methylcoumarin was synthesized from ethyl acetoacetate and m-dihydroxybenzene by the Pechmann condensation using phenyl sulfonic acid as catalyst under solvent-free conditions. Various affecting factors were investigated. When the amount of catalyst was about 0.5%(m-dihydroxybenzene,n/n),the mole ratio of ethyl acetoacetate to m-dihydroxybenzene was 1.3∶1,the yield reached to 85.0% under 110℃ in 21 min. The structure of the product was confirmed by IR. |
Key words:7-hydroxy-4-methylcoumarin;phenyl sulfonic acid;Pechmann condensation;synthesis
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基金項目:遼寧省教育廳資助項目(2007T108)。
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作者簡(jiǎn)介:張芳芳(1984-),女,山東濱州人,碩士研究生,研究方向:綠色化學(xué)與催化。(E-mail:zffabc@163.com)
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聯(lián) 系 人:姜 恒,教授。(E-mail:hjiang78@hotmail.com)
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收稿日期:2009-03-17
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