反应详情

温度

50 °C

To a solution of 5-chloro-6-(2,4,6-trifluorophenyl)-N-[(1S)-2,2,2-trifluoro-1-methylethyl][1,2,4]triazolo[1,5-a]pyrimidin-7-amine (600 mg, 1.5 mmol) and 3-dimethylamino-1-propanol (1.03 g, 10 mmol) in 5 mL of dimethylsulfoxide at room temperature is added sodium hydride (60% in mineral oil, 400 mg, 10 mmol). The mixture is heated at 50° C. for 30 min, and cooled to room temperature. Water is added to quench the reaction, and the product is extracted with ethyl acetate (x2). The combined organic extracts are washed with saturated sodium chloride (x4), dried over magnesium sulfate, and concentrated to a residue. The residue is chromatographed over silica gel, eluting with a gradient of ethyl acetate to 20% methyl alcohol in ethyl acetate. Concentration provides 5-chloro-6-{4-[3-(dimethylamino)propoxy]-2,6-difluorophenyl}-N-[(1S)-2,2,2-trifluoro-1-methylethyl][1,2,4]triazolo[1,5-a]pyrimidin-7-amine as a colorless oil (486 mg). MS: m/z 479.2 (M+H).

1. temperaturecooled to room temperature
2. customto quench
3. customthe reaction
4. extractionthe product is extracted with ethyl acetate (x2)
5. washThe combined organic extracts are washed with saturated sodium chloride (x4)
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated to a residue
8. customThe residue is chromatographed over silica gel
9. washeluting with a gradient of ethyl acetate to 20% methyl alcohol in ethyl acetate
10. concentrationConcentration