反应详情

A solution of 7-(3-methylsulphinylpropylamino)-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine (0.80 g) and m-chloroperoxybenzoic acid (0.40 g) in dichloromethane (50 ml) was stirred at ambient temperature for 24 hours. During this time further m-chloroperoxybenzoic acid (about 200 mg) was added on 2 occasions. The solution was washed with dilute aqueous sodium bicarbonate (3×25 ml) and the combined washings back-extracted with a little dichloromethane. The combined organic layer was washed with water and then brine, dried (magnesium sulphate) and evaporated under reduced pressure to yield a residue. This was recrystallised three times from methanol to yield the title compound, 0.51 g, m.p. 222°-3° C.

1. washThe solution was washed with dilute aqueous sodium bicarbonate (3×25 ml)
2. extractionthe combined washings back-extracted with a little dichloromethane
3. washThe combined organic layer was washed with water
4. dry with materialbrine, dried (magnesium sulphate)
5. customevaporated under reduced pressure
6. customto yield a residue
7. customThis was recrystallised three times from methanol