反应详情

In a oven dried 50 mL round bottom flask were sequentially added Compound 173 (620 mg, 1.69 mmol), 3-bromo-5-methylpyridin-2-amine (381 mg, 2.03 mmol), Pd2(dba)3 (77 mg, 0.08 mmol), xantphos (59 mg, 0.10 mmol) and NatBuO (244 mg, 2.53 mmol) at room temperature. The solid materials were kept under vacuum for 5 min. and then refilled with nitrogen. This process was repeated thrice before adding dry, degassed dioxane (8 mL). The heterogeneous mixture was stirred at room temperature for 15 min. and then at 100° C. for 2 h. Finally upon completion of the reaction, it was diluted with EtOAc and filtered through a small pad of silica gel with several washings. All the washings and filtrate concentrated in vacuum and the crude residue was further purified by flash chromatography to provide pure Compound 174 (574 mg, 80%).

1. customIn a oven dried 50 mL round bottom flask
2. customat room temperature
3. additionrefilled with nitrogen
4. additionbefore adding
5. customdry
6. customdegassed dioxane (8 mL)
7. waitat 100° C. for 2 h
8. customFinally upon completion of the reaction, it
9. filtrationfiltered through a small pad of silica gel with several washings
10. concentrationAll the washings and filtrate concentrated in vacuum
11. customthe crude residue was further purified by flash chromatography