反应详情

温度

60 °C

A mixture of 4-bromo-2-(2-chloro-6-fluorophenyl)-2H-pyrazolo[4,3-c]pyridine (166 mg, 0.51 mmol), tert-butyl carbamate (297 mg, 2.54 mmol), Pd2(dba)3 (23 mg, 0.025 mmol), Xantphos (29 mg, 0.05 mmol) and potassium phosphate tribasic (216 mg, 1.02 mmol) in toluene (5 mL) and water (1 mL) was degassed with argon then heated at 60° C. for 1.5 hours. The reaction mixture was cooled to room temperature and then filtered through Celite® washing with ethyl acetate. The filtrate was washed with water and brine, dried over magnesium sulfate and concentrated under reduced pressure. The resultant residue was purified by silica gel flash chromatography (0-35% ethyl acetate in cyclohexane) to afford the title compound as a yellow solid (137 mg, 74% yield). LCMS (Method C): RT=2.30 min, m/z: 348 [M−C4H7+].

1. customwas degassed with argon
2. temperatureThe reaction mixture was cooled to room temperature
3. filtrationfiltered through Celite®
4. washwashing with ethyl acetate
5. washThe filtrate was washed with water and brine
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe resultant residue was purified by silica gel flash chromatography (0-35% ethyl acetate in cyclohexane)