反应详情

温度

5 °C

1,3-Di-cyclopropylmethyl xanthine (20 g, 0.076 mol) was dissolved in acetic acid (33 ml) and then treated with concentrated nitric acid (13.2 g) at 87° C. After 1 hour, the mixture was cooled to 5° C. and the resulting yellow precipitate filtered off. The yellow crystals were dissolved in dichloromethane and washed with water. The separated organic layer was then dried over anhydrous sodium sulphate and concentrated in vacuo. The product crystallized from the concentrate to yield a yellow crystalline product yield 12.2 g, (56.5%), m.pt. 207° C. (with decomposition).

1. filtrationthe resulting yellow precipitate filtered off
2. dissolutionThe yellow crystals were dissolved in dichloromethane
3. washwashed with water
4. dry with materialThe separated organic layer was then dried over anhydrous sodium sulphate
5. concentrationconcentrated in vacuo
6. customThe product crystallized from the
7. concentrationconcentrate