反应详情

To a mixture of 4-cyano-2-methoxybenzoic acid (1.00 g, 5.648 mmol, Biogene) in methanol (15.0 mL) was added p-toluenesulfonic acid monohydrate (286 mg, 1.48 mmol, Aldrich) and it was heated to reflux under an argon atmosphere for 16 hrs. The solvent was removed and the reaction mixture was extracted with EtOAc, washed with saturated Na2CO3, water, and saturated NaCl. The organic phase was separated, dried over Na2SO4, filtered and concentrated to give 4-cyano-2-methoxy-benzoic acid methyl ester (1.04 g, 96.4%).

1. temperaturewas heated
2. temperatureto reflux under an argon atmosphere for 16 hrs
3. customThe solvent was removed
4. extractionthe reaction mixture was extracted with EtOAc
5. washwashed with saturated Na2CO3, water, and saturated NaCl
6. customThe organic phase was separated
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated