反应详情

To a solution of 3-hydroxy-2-methylbenzoic acid (3.80 g, 25.0 mmol) in methanol (3.0 mL) at 0° C. was added thionyl chloride (3.00 mL, 41.2 mmol) dropwise. The reaction was allowed to warm to room temperature and was then heated at 50° C. for 2 hours. The solvent was removed under vacuum and the resulting solids were dissolved in ethyl acetate and washed with NaHCO3 (sat. aq.). The ethyl acetate layer was dried over Na2SO4, filtered, and concentrated under vacuum to give methyl 3-hydroxy-2-methylbenzoate (114a, 3.49 g, 84% yield) as a light tan solid.

1. temperaturewas then heated at 50° C. for 2 hours
2. customThe solvent was removed under vacuum
3. dissolutionthe resulting solids were dissolved in ethyl acetate
4. washwashed with NaHCO3 (sat. aq.)
5. dry with materialThe ethyl acetate layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under vacuum