反応 #3725

反応方程式

1,3-Di-cyclopropylmethyl xanthine

nitric acid

→

product

収率 56.5%

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

収率 56.5%

溶媒

acetic acid

反応条件

後処理

1. 1
   ろ過the resulting yellow precipitate filtered off
2. 2
   workup.DISSOLUTIONThe yellow crystals were dissolved in dichloromethane
3. 3
   洗浄washed with water
4. 4
   乾燥The separated organic layer was then dried over anhydrous sodium sulphate
5. 5
   濃縮concentrated in vacuo
6. 6
   その他The product crystallized from the
7. 7
   濃縮concentrate

実験手順

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).

出典