HCID 21939176, compound → HCID 178432483, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 4-chloro-2-(2-chlorophenyl)-5,6-dimethylpyrimidine (31.14 g, 123 mmol) and 5-fluoro-1H-pyrazolo[3,4-b]pyridin-3-amine (19.65 g, 129 mmol) in NMP (200 mL) was heated at 135° C. for 3 h 30 min. Then the mixture was concentrated in vacuo to around 100 mL. Then added sat aq. NaHCO3, water and EtOAc but a precipitate appeared in the organic layer. Filtered off this whole mixture and washed the residue with sat aq. NaHCO3, water and EtOAc and ether. Boiling ethanol was added to the residue with stirring and the pure target compound was filtered. The liquors were concentrated and this trituration procedure repeated 4 times to give the target (25 g, 55%) as a white solid.

Provenance & Evidence