反応 #163
ord-f216b4e86bcc4a2b8660bf0c5e130be5
反応方程式
溶媒
反応条件
実験手順
2-chloro-4-iodo-5-(trifluoromethyl)pyridine (4.305 g, 14.00 mmol), 2-amino-N- methylbenzamide (2.103 g, 14.00 mmol), diacetoxypalladium (0.251 g, 1.12 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (1.296 g, 2.24 mmol) and cesium carbonate (5.47 g, 16.80 mmol) were mixed together in dioxane (80 mL). Reaction was degassed with argon and was stirred at 90 °C overnight (15 hours) under argon. Reaction was filtered, washed with CH2Cl2 and filtrate was concentrated to dryness. The crude product was purified by flash chromatography on silica gel eluting with 10 to 40% ethyl acetate in petroleum ether. The solvent was evaporated to dryness to afford 2-(2-chloro-5-(trifluoromethyl)pyridin-4-ylamino)-N-methylbenzamide (3.39 g, 73.4 %) as a white crystalline solid.