反应详情

60% NaH (0.14 mol) is added portionwise to a solution of 3-fluoro-4-formyl benzoic acid (3, 0.12 mol) in dry DMF (330 mL). The mixture is stirred at room temperature for 30 min. Methyl iodide (0.14 mol) is added dropwise to the mixture. After stirring at room temperature for 5 h, the reaction mixture is poured into 1 N HCl (ca. 1000 mL) and extracted twice with EtOAc. The combined organic layers are washed with saturated aqueous NaHCO3, brine, dried over MgSO4, and evaporated in vacuo to give crude 3-fluoro-4-formyl benzoic acid methyl ester (4).

1. stirringAfter stirring at room temperature for 5 h
2. extractionextracted twice with EtOAc
3. washThe combined organic layers are washed with saturated aqueous NaHCO3, brine
4. dry with materialdried over MgSO4
5. customevaporated in vacuo