反应详情

A mixture of 3 (2.41 g, 9.1 mmol), 5-aminosalicylic acid (1.40 g, 9.1 mmol) and glacial acetic acid (9 mL) was heated under reflux for 2 hours. After cooling, the precipitate was filtered and washed with acetic acid and water. The solid was recrystallized from acetic acid to afford 1.75 g (50% yield) title product as a yellow solid; MS m/z 380 (M−−H) 9.92 min; 1H NMR (DMSO-d6) δ 2.63 (t, 2H), 2.94 (t, 2H), 4.89 (s, 1H), 7.16 (m, 13H).

1. temperaturewas heated
2. temperatureunder reflux for 2 hours
3. temperatureAfter cooling
4. filtrationthe precipitate was filtered
5. washwashed with acetic acid and water
6. customThe solid was recrystallized from acetic acid