反应详情

A mixture of 3-(4-methoxy-2-phenoxy-phenylamino)-phthalic acid dimethyl ester (0.80 g, 2.0 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 CH2Cl2 (2×100 mL), and acidified (HCl). The resulting mixture was extracted with ethyl acetate (4×50 mL) and the combined extracts were washed with water (3×100 mL), dried (MgSO4) and evaporated, providing 0.69 g, in 93% yield; 1H NMR (DMSO-d6) δ 3.71 (s, 3H), 6.58 (d, J=2.7, 1H), 6.80 (dd, J=8.8 Hz, J=2.7 Hz, 1H), 6.88-6.94 (m, 3H), 7.03-7.10 (m, 2H), 7.27-7.36 (m, 4H), 8.07 (s, 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 CH2Cl2 (2×100 mL)
7. extractionThe resulting mixture was extracted with ethyl acetate (4×50 mL)
8. washthe combined extracts were washed with water (3×100 mL)
9. dry with materialdried (MgSO4)
10. customevaporated
11. customproviding 0.69 g