반응 #349
ord-879180a104c8430c87fe873fe28d1e66
용매
반응 조건
실험 절차
2-chloro-4-iodo-5-(trifluoromethyl)pyridine (0.502 g, 1.63 mmol), 2-amino-5-fluoro-N-methoxybenzamide (0.344 g, 1.68 mmol), diacetoxypalladium (0.029 g, 0.13 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.151 g, 0.26 mmol) and cesium carbonate (0.638 g, 1.96 mmol) were weighed out in a microwave vial and sealed. dioxane (10.31 ml) was added and argon was let to bubble through the reaction mixture then it was stirred at 90 °C for 5 hours. The reaction mixture was allowed to cool to room temperature, silca gel was added and the mixture was concentrated to afford the crude, which was purified by flash chromatography on silica gel eluting with 20 to 50% ethyl acetate in petroleum ether. The solvent was evaporated to dryness to afford 2-(2-chloro-5-(trifluoromethyl)pyridin-4-ylamino)-5-fluoro-N-methoxybenzamide (0.240 g, 40.4 %) as an yellow oil which crystallised on standing.