Reaktion #75385

Reaktionsgleichung

hydrogen peroxide

7,7-dimethyl-2-(2-methoxy-4-methylmercapto-phenyl)-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione

hydrogen peroxide

→

7,7-Dimethyl-2-(2-methoxy-4-methylsulfinyl-phenyl)-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione

Lösungsmittel

water

ammonia

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added until alkaline reaction
2. 2
   FiltrationThe precipitate was suction-filtered off
3. 3
   Extraktionthe filtrate was extracted twice with chloroform
4. 4
   SonstigeThe combined chloroform phases were evaporated
5. 5
   SonstigeThe thus obtained product was purified on a silicagel column (eluant: chloroform/acetone 19:1)

Vorschrift

5.1 gm of 7,7-dimethyl-2-(2-methoxy-4-methylmercapto-phenyl)-5H,7H-imidazo[4,5-h]isoquinoline-4,6-dione were reacted in 100 ml of 70% acetic acid with 1.7 gm of 30% hydrogen peroxide, and the mixture was allowed to stand for 50 hours at room temperature (the first 3 hours while stirring). After 18 and again after 26 hours 1.3 gm of 30% hydrogen peroxide were added. The reaction mixture was then diluted with water, and ammonia was added until alkaline reaction. The precipitate was suction-filtered off and the filtrate was extracted twice with chloroform. The combined chloroform phases were evaporated, and the evaporation residue was combined with the precipitate. The thus obtained product was purified on a silicagel column (eluant: chloroform/acetone 19:1).

Quelle