反应详情

A mixture of 3-(2,4-dimethoxyphenylamino)phthalic acid dimethyl ester (0.85 g, 2.5 mmol) and 3N NaOH (50 mL) in ethanol (100 mL) was heated to reflux for 90 minutes. The mixture was cooled, and the solvent was removed under vacuum. The residue was dissolved in water (100 mL), washed with ethyl acetate (3×75 mL), acidified (HCl) and extracted with ethyl acetate (3×75 mL). The combined organic extracts were washed with water (3×75 mL), dried (MgSO4), and evaporated, providing 0.76 g in 97% yield: 1H NMR (CDCl3) δ 3.82 (s, 3H), 3.84 (s, 3H), 6.52 (dd, J=8.6 Hz, J=2.5 Hz, 1H), 6.57 (d, J=2.5 Hz, 1H), 7.11 (d, J=8.6 Hz, 1H), 7.22-7.26 (m, 2H), 7.52 (t, J=7.8 Hz, 1H), 7.61 (br, 1H).

1. temperaturewas heated
2. temperatureto reflux for 90 minutes
3. temperatureThe mixture was cooled
4. customthe solvent was removed under vacuum
5. dissolutionThe residue was dissolved in water (100 mL)
6. washwashed with ethyl acetate (3×75 mL)
7. extractionextracted with ethyl acetate (3×75 mL)
8. washThe combined organic extracts were washed with water (3×75 mL)
9. dry with materialdried (MgSO4)
10. customevaporated
11. customproviding 0.76 g in 97% yield