反应详情

To a stirred solution of 3-[5-(2-amino-pyrimidin-5-yl)-1-tert-butyl-1H-benzimidazol-2-yl]-4-1,2,4-triazol-1-yl-phenol (100 mg, 0.23 mmol) in THF (3 mL) is added potassium carbonate (65 mg, 0.47 mmol) followed by isopropyl isocyanate (25 ul, 0.26 mmol). The resulting mixture is stirred at room temperature for 3 hours and then is warmed to 60° C. for 18 hours. The reaction is cooled to room temperature, poured into water and the product extracted into EtOAc (2×10 mL). The combined organics are dried with MgSO4 (500 mg), filtered, and concentrated. The remaining residue is purified by silica gel flash column chromatography (12 g silica gel, 0-5% MeOH/DCM). Product-containing fractions are combined and concentrated to give the title compound (15 mg, 13%). LCMS (ESMS): m/z 512.5 (M++1)

1. temperatureis warmed to 60° C. for 18 hours
2. temperatureThe reaction is cooled to room temperature
3. extractionthe product extracted into EtOAc (2×10 mL)
4. dry with materialThe combined organics are dried with MgSO4 (500 mg)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe remaining residue is purified by silica gel flash column chromatography (12 g silica gel, 0-5% MeOH/DCM)
8. concentrationconcentrated