反应详情

温度

160 °C

A mixture of 2-chloro-4-methoxy-phenol (Aldrich Chemical Company, Inc., Milwaukee, Wis., USA 29 mg, 0.178 mmol), 4-(4-chloro-pyrazolo[3,4-d]pyrimidin-1-yl)-piperidine-1-carboxylic acid tert-butyl ester (Intermediate 19; 60 mg, 0.178 mmol), and potassium carbonate (54 mg, 0.391 mmol) in dimethylformamide (1 mL) was heated in a microwave oven at 160° C. for 10 min. Saturated sodium carbonate solution was added to the reaction mixture, and the mixture was then filtered through a pad of silica gel to remove the precipitate. The silica gel pad was washed with methanol and the solvents were evaporated from the filtrate. The residue was purified by HPLC to afford 4-[4-(2-chloro-4-methoxy-phenoxy)-pyrazolo[3,4-d]pyrimidin-1-yl]-piperidine-1-carboxylic acid tert-butyl ester (28 mg, 34%) as a white solid. Mass spectrum MH+=460.

1. filtrationthe mixture was then filtered through a pad of silica gel
2. customto remove the precipitate
3. washThe silica gel pad was washed with methanol
4. customthe solvents were evaporated from the filtrate
5. customThe residue was purified by HPLC