Reaktion #3724

Reaktionsgleichung

1,3-Di-n-butylxanthine

nitric acid

→

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

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationthe resulting yellow precipitate filtered off
2. 2
   Waschenwashed with water (50 ml)
3. 3
   workup.DISSOLUTIONThe yellow crystals were dissolved in dichloromethane
4. 4
   Waschenwashed twice with water
5. 5
   TrocknenThe separated organic layer was then dried (anhydrous sodium sulphate)
6. 6
   Einengenconcentrated
7. 7
   Sonstigeto give a crystalline product, yield 73 g (86%), m.pt 168° C.

Vorschrift

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.

Quelle