2-amino-6-methoxy-N-methylbenzamide → 2-[[2-[(1,3-dimethylpyrazol-4-yl)amino]-5-(trifluoromethyl)-4-pyridyl]amino]-6-methoxy-N-methyl-benzamide

温度

100 °C

A suspension of [Reactants], N-(1,3-dimethyl-1H-pyrazol-4-yl)-4-iodo-5-(trifluoromethyl)pyridin-2-amine (2.63 g, 6.88 mmol), diacetoxypalladium (0.077 g, 0.34 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.398 g, 0.69 mmol) and cesium carbonate (4.48 g, 13.77 mmol) in dioxane (37 mL) was degassed with argon then stirred at 100 °C for 3 hours . The reaction mixture was concentrated to dryness, diluted with ethyl acetate (80 ml), washed with water (1 x 50 ml), brine, dried over magnesium sulfate and concentrated to afford an oil. The crude product was purified by flash chromatography on silica gel eluting with AcOet pure to remove impurities then 3 to 8% methanol in ethyl acetate. The solvent was evaporated to dryness to afford a foam which was dissolved in dichloromethane ( 12ml ). A solid was formed after a few minutes, which was filtered, dried .A white solid was obtained 2-(2-(1,3-dimethyl-1H-pyrazol-4-ylamino)-5-(trifluoromethyl)pyridin-4-ylamino)-6-methoxy- N-methylbenzamide (1.570 g, 52.5 %)

ORDレコード

ord-183f397304e242fab1c88325fcefdf27

出典データセット

750 AstraZeneca ELN dataset

元リンク

出典を表示