反应详情

温度

50 °C

Thionyl chloride (953 μL, 13.1 mmol) was added dropwise to a solution of 4-hydroxy-2-methoxy-benzoic acid (733 mg, 4.36 mmol) in methanol (30 mL) at 0° C. The mixture was stirred at 50° C. overnight. The reaction mixture was concentrated and the residue was dissolved in water (40 mL). The solution was neutralized with saturated sodium bicarbonate solution and the product was extracted into ethyl acetate. The organics were dried over sodium sulfate, filtered and evaporated to dryness to give methyl 4-hydroxy-2-methoxy-benzoate (99%). ESI-MS m/z calc 182.1. found 183.1 (M+1)+. Retention time: 0.73 minutes (3 min run).

1. concentrationThe reaction mixture was concentrated
2. dissolutionthe residue was dissolved in water (40 mL)
3. extractionthe product was extracted into ethyl acetate
4. dry with materialThe organics were dried over sodium sulfate
5. filtrationfiltered
6. customevaporated to dryness