反应详情

A mixture of 2-methyl-5-(3-methyl-[1,2,4]oxadiazol-5-yl)-phenol (72.0 mg, 0.0.379 mmol) and potassium carbonate (64.2 mg, 0.455 mmole) in dimethylformamide was stirred at room temperature for 30 minutes before 3-bromomethyl-4-chloro-1-methyl-1H-pyrazolo[3,4-d]pyrimidine (89.8 mg, 0.280 mmol, Example 5) was added. The reaction was stirred at room temperature overnight and then concentrated under reduced pressure to remove dimethylformamide. The residue was dissolved in ethyl acetate, washed with water, dried and concentrated. The crude product was purified by flash chromatography (silica gel, hexanes-ethyl acetate, 90/10 to 60/40) to give pure 4-chloro-1-methyl-3-[2-methyl-5-(3-methyl-[1,2,4]oxadiazol-5-yl)-phenoxymethyl]-1H-pyrazolo[3,4-d]pyrimidine as a white solid. (Yield 41.0 mg).

1. additionwas added
2. concentrationconcentrated under reduced pressure
3. customto remove dimethylformamide
4. dissolutionThe residue was dissolved in ethyl acetate
5. washwashed with water
6. customdried
7. concentrationconcentrated
8. customThe crude product was purified by flash chromatography (silica gel, hexanes-ethyl acetate, 90/10 to 60/40)