反应详情

温度

60 °C

Potassium tert-butoxide (84 mg) was added to 5-[(1-methyl-4-phenyl-1H-imidazol-5-yl)ethynyl]pyrimidin-4-amine (intermediate 28) (41 mg) stirred in NMP (2 mL) and heated to 60° C. for 5 hours. After cooling to ambient temperature, water (3 mL) and then DCM (10 mL) was added. The reaction mixture was washed with water (4×10 mL), dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica eluting with DCM:MeOH (20:1 to 10:1) afforded the title compound as a white solid (13.6 mg, 33%);

1. temperatureAfter cooling to ambient temperature
2. washThe reaction mixture was washed with water (4×10 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification by flash chromatography on silica eluting with DCM:MeOH (20:1 to 10:1)