反应 #3725

反应方程式

1,3-Di-cyclopropylmethyl xanthine

nitric acid

→

product

收率 56.5%

1,3-Di-cyclopropylmethyl-8-nitro Xanthine

收率 56.5%

溶剂

acetic acid

反应条件

后处理

1. 1
   过滤the resulting yellow precipitate filtered off
2. 2
   workup.DISSOLUTIONThe yellow crystals were dissolved in dichloromethane
3. 3
   洗涤washed with water
4. 4
   干燥The separated organic layer was then dried over anhydrous sodium sulphate
5. 5
   浓缩concentrated in vacuo
6. 6
   其他The product crystallized from the
7. 7
   浓缩concentrate

实验过程

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).

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