反应详情

温度

110 °C

To a solution of 7-chloro-2-(4-methoxybenzyl)-3,4-dihydro-1H-pyrido[1,2-a]pyrazine-1,6-(2H)-dione (3, 0.45 g, 1.41 mmol) in dioxane (10 mL), pyrimidin-4-amine (4, 0.13 g, 1.41 mmol), sodium tert-butoxide (0.41 g, 4.2 mmol) followed by X-Phos (0.14 g, 0.28 mmol) were added and the reaction mixture was degassed with argon for 5 min. Tris(dibenzylideneacetone)dipalladium(0) (0.13 g, 0.14 mmol) was added and the reaction mixture was degassed with argon for another 5 min and stirred at 110° C. for 16 h. The reaction mixture was diluted with water and the compound was extracted in ethyl acetate. The organic layer was washed with brine, separated, dried over sodium sulphate and concentrated under reduced pressure. The residue obtained was purified via column chromatography (silica, methanol/dichloromethane=5%) to afford 2-(4-methoxybenzyl)-7-(pyrimidin-4-ylamino)-3,4-dihydro-1H-pyrido[1,2-c]pyrazine-1,6(2H)-dione (5) as a yellow solid. Yield: 0.42 g, 79%; MS (ESI) m/z 378 [M+1]+.

1. additionwere added
2. customthe reaction mixture was degassed with argon for 5 min
3. customthe reaction mixture was degassed with argon for another 5 min
4. additionThe reaction mixture was diluted with water
5. extractionthe compound was extracted in ethyl acetate
6. washThe organic layer was washed with brine
7. customseparated
8. dry with materialdried over sodium sulphate
9. concentrationconcentrated under reduced pressure
10. customThe residue obtained
11. customwas purified via column chromatography (silica, methanol/dichloromethane=5%)