反应详情

To a solution of (3S,6R)-6-methyl-N-phenyl-3-piperidinecarboxamide (12 g, 55 mmol) in 1,4-dioxane (250 mL) was added 4,6-dichloro-2-pyrimidinamine (8.11 g, 49.5 mmol) and sat. aqueous NaHCO3 (125 mL), and the reaction mixture was then refluxed overnight. The reaction was not completed. The reaction mixture was cooled, added 4,6-dichloro-2-pyrimidinamine (0.9 g, 5.5 mmol), and refluxed overnight. When the reaction was completed, the mixture was cooled down. To the mixture was added about 500 mL of H2O to form a precipitate, and then filtered to obtain a gummy solid. The gummy solid was then dissolved in EtOAc (˜800 mL). The organic solution was washed with water (2×200 mL), brine (200 mL), dried (Na2SO4), filtered, and concentrated in vacuo to afford the crude title compound (20 g). LC-MS (ES) m/z=346 [M+H]+.

1. temperaturethe reaction mixture was then refluxed overnight
2. temperatureThe reaction mixture was cooled
3. temperaturerefluxed overnight
4. temperaturethe mixture was cooled down
5. customto form a precipitate
6. filtrationfiltered
7. customto obtain a gummy solid
8. washThe organic solution was washed with water (2×200 mL), brine (200 mL)
9. dry with materialdried (Na2SO4)
10. filtrationfiltered
11. concentrationconcentrated in vacuo