Methanol → HCID 86624325, compound

Participants

Reaction Conditions

Reaction Steps

Charge 1-(5-tert-butyl-2-p-tolyl-2H-pyrazol-3-yl)-3-{6-[4-(2,6-difluoro-benzoyl)-piperazin-1-yl]-2-methyl-pyridin-3-yl}-urea (1.00 equiv, 600.67 mmol, 353.00 g), and methanol (3.50 L) to a 5 L flask. Heat the mixture was to 50-60° C. Add methanesulfonic acid (1.00 equiv, 603.49 mmol, 39.56 mL, 58.00 g) in 250 mL of ethyl acetate drop wise. Stir the solution for 0.5 hour at ˜50° C., then remove heating source. Stir for 5 hours, then filter. Concentrate filtrate under reduced pressure. Add ethyl acetate (300 mL) and concentrate under reduced pressure. Add an additional 300 mL of ethyl acetate was added concentrate under reduced pressure. Add 2 L of diethyl ether then stir for 15 minutes. Allow to stand overnight. Stir for 3 hours then filter. Rinse diethyl ether and heptane, then dry under reduced pressure at ˜40° C. to afford the title compound (391.4 g).

Provenance & Evidence