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A solution of dimethyl-4-hydroxyisophthalate (10.0 g, 47.6 mmol) in pyridine (70 mL) was heated to reflux for 15 h. The reaction mixture was concentrated in vacuo and acidified with 1N HCl at 0° C. The resulting solid was collected by filtration, washed with water and dried in vacuo to provide the title compound (9.3 g, 100%) as a white solid. 1H NMR (DMSO-d6) δ 8.40 (d, J=2.0 Hz, 1H), 8.06 (dd, J=8.4, 2.0 Hz, 1H), 7.07 (d, J=8.4 Hz, 1H), 3.84 (s, 3H); MS(ESI−) m/z 195.2 (M−H)−.

1. temperatureto reflux for 15 h
2. concentrationThe reaction mixture was concentrated in vacuo
3. customacidified with 1N HCl at 0° C
4. filtrationThe resulting solid was collected by filtration
5. washwashed with water
6. customdried in vacuo