反应详情

温度

100 °C

A microwave tube was charged with a stir bar, N-(2,6-dibromopyridin-4-yl)acetamide (0.95 g, 3.23 mmol), 2-Amino-4-(trifluoromethyl)pyridine (0.576 g, 3.56 mmol), Pd(OAc)2 (0.073 g, 0.323 mmol), Xantphos (0.281 g, 0.485 mmol), and Cs2CO3 (2.106 g, 6.46 mmol). The mixture was vacuum-purged with argon 3 times, then degassed dioxane (6.46 mL) was added. The reaction was sealed and heated to 100° C. for 3 hours, after which time the reaction was cooled to rt, diluted with MeOH (10 mL) and concentrated under reduced pressure. The product was purified by silica gel chromatography using a gradient solvent system of 0-100% EtOAc/Hexanes. The product containing fractions were collected and concentrated to give N-(2-bromo-6-((4-(trifluoromethyl)pyridin-2-yl)amino)pyridin-4-yl)acetamide (605 mg, 50%) as a white solid. MS ESI calcd for C13H10BrF3N4O [M+H]+ 375, found 375.

1. additionA microwave tube was charged with a stir bar
2. customThe mixture was vacuum-purged with argon 3 times
3. additiondegassed dioxane (6.46 mL) was added
4. customThe reaction was sealed
5. temperatureafter which time the reaction was cooled to rt
6. additiondiluted with MeOH (10 mL)
7. concentrationconcentrated under reduced pressure
8. customThe product was purified by silica gel chromatography
9. additionThe product containing fractions
10. customwere collected
11. concentrationconcentrated