Реакция #75385

Уравнение реакции

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

Растворители

water

ammonia

acetic acid

Условия реакции

Обработка

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

Методика

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).

Источник