反应详情

温度

60 °C

A suspension of 0.2261 g (0.65 mmol) of 3-(3,5-dimethoxy-phenyl)-7-methanesulfinyl-3,4-dihydro-pyrimido[4,5-d]pyrimidin-2(1H)-one and 0.103 g (0.71 mmol) of diethylaminobutylamine in 10 mL of dry dioxane was warmed to 60° C. and stirred overnight. To the reaction mixture was added 0.306 g (2.13 mmol) of diethylaminobutylamine and 0.1658 g (0.71 mmol) of camphorsulfonic acid. The reaction mixture was stirred for another 18 hours at 60° C. The reaction solution was concentrated in vacuo, and the residue was partitioned between ethyl acetate and a saturated solution of sodium bicarbonate. The ethyl acetate layer was washed with a saturated solution of sodium bicarbonate, then with water, dried over magnesium sulfate, and concentrated in vacuo. The residue was chromatographed down silica gel, eluting with ethyl acetate/ethanol/triethylamine (9:2:1 v/v/v) to give 0.173 g (62%) of the title compound: mp 203-207° C.

1. stirringThe reaction mixture was stirred for another 18 hours at 60° C
2. concentrationThe reaction solution was concentrated in vacuo
3. customthe residue was partitioned between ethyl acetate
4. washThe ethyl acetate layer was washed with a saturated solution of sodium bicarbonate
5. dry with materialwith water, dried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was chromatographed down silica gel
8. washeluting with ethyl acetate/ethanol/triethylamine (9:2:1 v/v/v)