反应详情

温度

100 °C

A suspension of [Reactants], N-(1,3-dimethyl-1H-pyrazol-4-yl)-4-iodo-5-(trifluoromethyl)pyridin-2-amine (150 mg, 0.39 mmol), diacetoxypalladium (4.41 mg, 0.02 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (22.71 mg, 0.04 mmol) and cesium carbonate (256 mg, 0.79 mmol) in dioxane (2 mL) was degassed with argon then stirred at 100 °C for 2 hours sealed in a microwave vial. The reaction mixture was purified by preparative HPLC using a Waters X-Bridge reverse-phase column (C-18, 5 microns silica, 19 mm diameter, 100 mm length, flow rate of 40 ml / minute) and decreasingly polar mixtures of water (containing 0.2% ammonium carbonate) and acetonitrile as eluent. The fractions containing the desired compound were evaporated to dryness to afford impure product EN01775-26-01. The impure product was repurified by flash chromatography on silica gel eluting with 0 to 5% methanol in ethyl acetate/DCM (1/1) - spillage occurred when collecting. The solvent was evaporated to dryness to afford 110mg of a foam, which was triturated in tBuOMe. The resulting precipitate was collected by filtration and dried to a constant weight to afford [Products] as a white solid EN01775-26-02 (81 mg, 0.186 mmol, 47.5 %).