反应详情

4.9 g of 4-chloro-6-methylthio-pyrimido[5,4-d]pyrimidine, 2.0 g of 3-methylaniline, 2.4 ml of triethylamine and 100 ml of dioxane are heated at 100° C. for 3 hours. After cooling, the reaction mixture is concentrated and partitioned between water and methylene chloride. The organic phase is separated off, dried and concentrated and the residue is purified by chromatography over a silica gel column (petroleum ether/ethyl acetate=2:1). The solid is triturated with diethyl ether, filtered off with suction and dried.

1. temperatureAfter cooling
2. concentrationthe reaction mixture is concentrated
3. custompartitioned between water and methylene chloride
4. customThe organic phase is separated off
5. customdried
6. concentrationconcentrated
7. customthe residue is purified by chromatography over a silica gel column (petroleum ether/ethyl acetate=2:1)
8. customThe solid is triturated with diethyl ether
9. filtrationfiltered off with suction
10. customdried