反应详情

To a solution of 4-methoxy-2-nitrobenzoic acid (12 g; 61 mmol; 1 eq; commercially available from Aldrich) in MeOH (200 mL) is added thionyl chloride (13 mL, 178 mmol, 2.9 eq) and the mixture is stirred at room temperature for 15 h. The solvent is removed under vacuum and the residue is diluted with EtOAc (150 mL) and washed with a 10% aqueous solution of sodium bicarbonate, water, and then dried over MgSO4. The solvent is removed under reduced pressure to afford 11 g (85%) of the title compound as a white solid. 1H NMR (CDCl3, 400 MHz) δ 7.81-7.79 (m, 1H), 7.27-7.25 (m, 1H), 7.13-7.11 (m, 1H), 3.92 (s, 3H), 3.89 (s, 3H).

1. customThe solvent is removed under vacuum
2. additionthe residue is diluted with EtOAc (150 mL)
3. washwashed with a 10% aqueous solution of sodium bicarbonate, water
4. dry with materialdried over MgSO4
5. customThe solvent is removed under reduced pressure