反应详情

温度

65 °C

To a solution of 5-hydroxyanthranilic acid (46.0 g, 300 mmol) in p-dioxane was added 1.93 M phosgene in toluene (186 mL, 360 mmol) and the resulting mixture stirred for 30 min. The mixture was heated at 65° C. for 4 h. After cooling, 1 N aqueous hydrochloric acid (150 mL) was added and the mixture stirred vigorously. The resulting precipitate was filtered and vacuum dried at 70° C./0.1 mm for 14 h to give 40.7 g (76%) of the title compound as a gray solid.

1. temperatureAfter cooling
2. stirringthe mixture stirred vigorously
3. filtrationThe resulting precipitate was filtered
4. customvacuum dried at 70° C./0.1 mm for 14 h