反应详情

温度

65 °C

Trimethylaluminum (23.9 mL, 47.8 mmol, 2M sol. in toluene) was added to a vigorously stirred solution of 7-chloro-1H-pyrazolo[3,4-c]pyridine (3.67 g, 23.9 mmol) and Pd(PPh3)4 (1.38 g, 1.19 mmol) in THF (109 mL) under argon. The reaction mixture was stirred at 65° C. for 16 h. The mixture was cooled to RT and poured into sat. aq. NH4Cl. The resulting suspension was filtered, the solid washed with water and discarded. The filtrate and the combined washings were extracted with EtOAc (3×). The combined organic extracts were washed with brine then dried (Phase separator) and concentrated under reduced pressure to give 7-methyl-1H-pyrazolo[3,4-c]pyridine as a solid. MS (LC-MS): 134 [M+H]+, tR (HPLC conditions k): 0.25 min.

1. temperatureThe mixture was cooled to RT
2. filtrationThe resulting suspension was filtered
3. washthe solid washed with water
4. extractionThe filtrate and the combined washings were extracted with EtOAc (3×)
5. washThe combined organic extracts were washed with brine
6. customthen dried (Phase separator)
7. concentrationconcentrated under reduced pressure