반응 #293
ord-62ffd954c4be4ad5b0533c19b263b236
용매
반응 조건
실험 절차
2-amino-6-methoxy-N-methylbenzamide (19.45 g, 107.95 mmol), N-(1,3-dimethyl-1H-pyrazol-5-yl)-4-iodo-5-(trifluoromethyl)pyridin-2-amine (27.5 g, 71.97 mmol) (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (4.16 g, 7.20 mmol) diacetoxypalladium (0.808 g, 3.60 mmol) and cesium carbonate (42.2 g, 129.54 mmol) were suspended in dioxane (300 mL). The reaction was degased, purged with argon sereval times and heated to 95 °C overnight. The reaction mixture was allowed to cool to rt, the insolubles were removed by filtration, washed with EtOAc and the filtrate was concentrated. The resulting residue was triturated with dichloromethane (150 ml), filtered, washed with DCM to give EN03299-47-01 (8.5 g, 19.57 mmol, 27.2 %) The filtrate was purified by flash chromatography on silica gel eluting with AcOEt and 5% methanol in ethyl acetate. Solvent were evaporated. The resulting precipitate was collected by filtration, washed with dichloromethane and dried to afford EN03299-47-02 (4.5 g, 10.36 mmol, 14.39 %). Not enought combined with _EN03299-49_