Synthesis of 4-ethoxy-7-hydroxycoumarin and its derivatives | 4-乙氧基-7-羟基香豆素及其衍生物的合成
2009
Zhang Weihua, Nanjing Agricultural University, Nanjing(China), College of Sciences | Bu Wenan, Nanjing Agricultural University, Nanjing(China), College of Sciences | Ma Chen, Nanjing Agricultural University, Nanjing(China), College of Sciences
中国人. 以间二酚和氰基乙酸为主要原料，经Pechmann反应、水解、乙醚化、Williamson反应合成了9种7烷氧基-4-乙氧基香豆素类新化合物。Williamson反应的优化条件为：N，N-二甲基甲酰胺（DMF）为溶剂，n（4-乙氧基-7羟基香豆素）：n（卤代烃）：n（碳酸钾）：n（TBAB，四正丁基溴化铵）=1：1．5：2．5：0．1，60～80℃反应11～25h，产率为72％～95％。中间产物及目标产物结构经红外光谱（IR）、质谱（MS）、核磁共振氢谱（. HNMR）表征得以证实。[著者文摘]
显示更多 [+] 显示较少 [-]英语. Nine new 7-alkoxy-4-ethoxycoumarins were synthesized from resorcinol and cyanoacetic by Pechmann reaction, hydrolyzation, ethyl etherization, and Williamson reaction. Optimum conditions for Williamson reaction were presented. In DMF （dimethylformamide）, when n （4-ethoxy-7-hydroxycoumarin） ：n （alkylhalides） ：n （anhydrous potassium carbonate） ：n （TBAB, tetrabutyl ammonium bromide） = 1 ： 1.5： 2. 5： 0. 1 and they were reacting at 60 ℃ to 80 ℃ for 11 h to 25 h, the yields were between 72%-95%. The structure of the intermediates and the target compounds were confirmed by IR, MS and . H NMR.
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