preparation | 3.32g(0.02mol) of 2,5-dimethoxybenzaldehyde, 0.5g of ammonium acetate and 4mL of nitromethane are put into a reaction bottle together, heated to 85 ℃ under stirring, kept warm for 30min, poured the reactant into cold water while hot, cooled, precipitated yellow crystals, filtered, washed with 70% ethanol to obtain 2,5-dimethoxy-β-nitrostyrene 3.7g (yield 90%). add 4.18g of 2,5-dimethoxy-β-nitro styrene into a 250mL three-neck bottle, add 20mL of 95% ethanol, stir, heat to 40 ℃, add 35mL of concentrated hydrochloric acid and 40mL of water; Add 25g of zinc powder in batches at 65 ℃, add a small amount of zinc powder, add a small amount of metal mercury, and keep the temperature between 65 and 70 ℃; Add zinc powder, cool to 50 ℃, add 10mL of hydrochloric acid, maintain 50~55 ℃ for 3h; Cooling, adding sodium carbonate to adjust pH8 ~ 9, extracting with n-butanol, distilled under reduced pressure to remove n-butanol from the extract, and the reactants turn into dark brown paste, weighing 6.5g. Salt formation: add methanol hydrochloric acid solution to the slurry reactant, evaporate most of the methanol, cool and precipitate to obtain light brown crystal 2,5-dimethoxy-β-nitrostyrene, 2.52g (yield 60%). |