preparation | 250ml three-neck bottle was added with ethyl 3, 4-dimethoxyacetophenone (17.9g,0.075mol), ethylene glycol (60ml) and 85% hydrazine hydrate (22.1g,0.375mol), slowly heated to 120 ℃ for 2h. After cooling to room temperature, add potassium hydroxide (12.6g,0.225mol), heat to 180 ℃, evaporate low boiling matter (about 2h) while heating, and then reflow for 4h. After the reaction, cool to room temperature, add 6mol/L hydrochloric acid (about 30ml) to pH2 ~ 3. Add water (150ml), extract with ethyl acetate (50ml × 4), and combine the organic phase. After washing with water (50ml × 2), it is dried by anhydrous sodium sulfate and then filtered, the filtrate is concentrated to dry under reduced pressure, and the remainder is recrystallized with ethyl acetate-petroleum ether (1:1) to obtain a white solid 3, 4-dimethoxyphenylacetic acid (10.8g,73.4%). 3, 4-dimethoxyphenylacetic acid and methanol esterification condensation, the target product 3, 4-dimethoxyphenylacetate methyl ester. |