10242-08-7, 5-Methoxybenzofuran-2-carboxylic acid is a benzofuran compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
Under ice-cooling,2-hydroxy-5-methoxybenzaldehyde (3.0g, 20mmol) and anhydrous K2CO3 (3.3g,23.4mmol) (50ml) was dissolved in DMF, was slowly added dropwise ethylbromoacetate (3.3g, 20mmol). After dropping Bi, 0 C was stirred for 30min,then at 60 C in an oil bath, the reaction 12h. The reaction solution waspoured into ice water, over Filtered, the solid was dissolved in chloroform,dried over anhydrous Na2SO4, filtered, and spin dry the solvent, by silica gelcolumn chromatography, To give 3.24 g of a yellow solid (75% yield), which was dissolved indioxane (30ml) was added 1N hydrogen Sodium hydroxide solution (15ml), stirredat room temperature 2h, the dioxane was evaporated to dryness, the residualliquid was poured into ice water, washed with diethyl Washed with methylenechloride, adjusting the PH value to 2, the solid was collected by filtration 2.68g (92% yield), whichwas dissolved in methylene Dioxane (50ml), was added DIC (1.51g, 11.98mmol),after stirring at room temperature 1h, was added DMAP (0.24g, 1.96 mmol) anddimethyl hydroxyethyl phosphonate (1.84g, 10.95mmol), heated to reflux after6h, water and saturated brine The reaction solution was washed with water,dried over anhydrous magnesium sulfate, filtered and evaporated to dryness,ethyl acetate – petroleum ether system recrystallized To (dimethoxyphosphoryl)ethyl 5-methoxybenzofuran-2-carboxylate 3.67g (77% yield), which was Was dissolved indichloromethane (50ml), was added trimethylsilyl bromide (9.85g, 64.8mmol) atroom temperature was stirred for 3h, with Quench with methanol, evaporated todryness to give the product 5-methoxy-benzofuran-2-carboxylic acid ethyl esterphosphono 2.38 g (yield, 74%)., 10242-08-7
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Reference£º
Patent; Institute of Medicinal Biotechnology Chinese Academy of MedicalSciences; Li, Zhuorong; Liu, Zongying; Xue, Situ; He, Xiaobo; Jin, Jie; Si, Shuyi; Ye, Weidong; (43 pag.)CN103130705; (2016); B;,
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