反应详情

To a solution of 2-chloro-4-hydroxybenzoic acid hydrate (2.0 g, 12 mmol), iodomethane (2.9 mL, 46 mmol) and N,N-dimethylformamide (50 mL) was added sodium hydride (1.9 g, 46 mmol; 60% dispersion in mineral oil) in one portion. After stirring the mixture vigorously for 16 h, the reaction was quenched with water and washed with ethyl acetate. The aqueous layer was then acidified with aqueous hydrogen chloride (6N) to give a white precipitate. The mixture was filtered, washed with water, and the filter cake was dried in a vacuum oven to give the desired acid as an off-white solid (1.4 g, 65%). MS (ESI) 187.1, 189.1 (M+H).

1. customthe reaction was quenched with water
2. washwashed with ethyl acetate
3. customto give a white precipitate
4. filtrationThe mixture was filtered
5. washwashed with water
6. customthe filter cake was dried in a vacuum oven