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机构地区:[1]天津理工大学化学化工学院,天津300384 [2]天津生物工程职业技术学院,天津300462
出 处:《精细石油化工》2014年第5期67-70,共4页Speciality Petrochemicals
摘 要:以间苯二酚/地衣酚和β-酮酸酯为原料,以1.2倍物质的量的蜜胺甲醛树脂(MF)负载硫酸为催化剂,在微波功率800W,辐射时间5~8min条件下,通过Pechmann缩合反应制备了4-甲基-7-羟基香豆素-3-脂肪酸乙酯,采用IR、1 H NMR和元素分析等分析手段对其结构进行了表征。结果表明:该催化剂具有良好的催化性能,可多次使用,合成收率达到85%~93%。A convenient procedure for the synthesis of ethyl 7-hydroxy-4-methyl coumarin-3-acids via Pechmann condensation by the same molar ratios of phenols with fi-keto esters using 1.2 times molar of melamine formaldehyde resin (MF) supported sulfuric acid as dehydration reagent under micro- wave-accelerated condition at the power of 800 W in 5--8 m has been developed. Structures of the corresponding products were characterized by IR, 1HNMR spectra and elemental analysis. Results showed that this catalyst can be recovered and recycled up to several consecutive runs after activation with yield of 85 %-93%, which will play a vital role in the process of Pechmann reaction.
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