反応 #3724

反応方程式

1,3-Di-n-butylxanthine

nitric acid

→

1,3-Di-n-butyl-8-nitro Xanthine

溶媒

acetic acid

反応条件

後処理

1. 1
   ろ過the resulting yellow precipitate filtered off
2. 2
   洗浄washed with water (50 ml)
3. 3
   workup.DISSOLUTIONThe yellow crystals were dissolved in dichloromethane
4. 4
   洗浄washed twice with water
5. 5
   乾燥The separated organic layer was then dried (anhydrous sodium sulphate)
6. 6
   濃縮concentrated
7. 7
   その他to give a crystalline product, yield 73 g (86%), m.pt 168° C.

実験手順

1,3-Di-n-butylxanthine (73 g, 0.28 mol) was dissolved in acetic acid (120 ml) and then treated with concentrated nitric acid (49 g) at 87° C. After 1 hour, the mixture was cooled to 5° C., the resulting yellow precipitate filtered off and washed with water (50 ml). The yellow crystals were dissolved in dichloromethane and washed twice with water. The separated organic layer was then dried (anhydrous sodium sulphate) and concentrated to give a crystalline product, yield 73 g (86%), m.pt 168° C.

出典