反应详情

温度

120 °C

Palladium (II) acetate (0.21 g, 0.31 mmol) and 2-Dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl (X-phos) (0.36 g, 0.75 mmol) were combined in toluene and heated at 120° C. for 3 min in microwave reactor. To this mixture tert-butyl 3-amino-2,6-dichloropyridin-4-ylcarbamate 2.43 (0.87 g, 3.12 mmol), Cs2CO3 (3.06 g, 9.38 mmol) and methyl iodide (0.196 mL, 3.12 mmol) were added and heated at 90° C. for 2 hr in a microwave reactor. After completion of the reaction, solvent was removed under reduced pressure. Solids were dissolved and extracted with ethyl acetate and water. Organic layer was washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The residue obtained was heated in acetonitrile and solids were filtered out to obtain tert-butyl 2,6-dichloro-3-(methylamino)pyridin-4-ylcarbamate 2.44 that was used for next step without further purification.

1. temperatureheated at 90° C. for 2 hr in a microwave reactor
2. customAfter completion of the reaction, solvent
3. customwas removed under reduced pressure
4. dissolutionSolids were dissolved
5. extractionextracted with ethyl acetate and water
6. washOrganic layer was washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe residue obtained
11. filtrationsolids were filtered out