反应详情

To a suspension of the product of example 1 (300 g, 1.21 mol) in 3 L of acetic acid, nitric acid (255 mL, ca. 6 mol, fuming, 90%) is added over 30 min at room temperature. Yellow precipitate is formed within minutes and increases over time. The reaction is kept at room temperature for 18 hours, before it is poured into 6 L of water. After stirred for 2 hours, the yellow suspension is filtered. The precipitate is washed with water (1.5 L×3) and EtOH (0.5 L×2) and dried in oven at 50° C. overnight to give 333 g (94%) of the title compound as a solid.

1. additionis added over 30 min at room temperature
2. customYellow precipitate is formed within minutes
3. temperatureincreases over time
4. filtrationthe yellow suspension is filtered
5. washThe precipitate is washed with water (1.5 L×3) and EtOH (0.5 L×2)
6. customdried in oven at 50° C. overnight