Ethanol → 1H-Pyrazolo[3,4-b]pyridine-3-carboximidamide, 5-fluoro-1-[(2-fluorophenyl)methyl]-, hydrochloride (1:1)

Participants

Reaction Steps

406.0 g (1.50 mol) of the compound from Example 8 were suspended in 2.081 of ethanol. Subsequently, 54.1 g (0.30 mol) of sodium methoxide in methanol (30%) were added and the mixture was stirred at room temperature overnight. 88.4 g (1.65 mol) of ammonium chloride were added, and the mixture was heated to 65° C. and stirred at 65° C. for 3.5 h. The solvents were distilled off and the residue was stirred with 1.61 of ethyl acetate overnight. The precipitated solids were filtered off with suction, washed twice with 140 ml each time of ethyl acetate and dried in a vacuum drying cabinet at 50° C. under a gentle nitrogen stream. This gave 441.4 g (90.7% of theory) of the title compound.

Provenance & Evidence