反应详情

Treat a 22° C. solution of 4-{5-[3-(5-tert-butyl-2-p-tolyl-2H-pyrazol-3-yl)-ureido]-6-methyl-pyridin-2-yl}-piperazine-1-carboxylic acid tert-butyl ester (Preparation 49; 63.20 g, 115.4 mmol) in MeOH (600 mL) with HCl (4 N solution in dioxane, 300 mL, 1200 mmol). Stir the mixture for 4 hours then concentrate under reduced pressure (room temperature, ca. 10 torr, 3 days) to afford 1-(5-tert-butyl-2-p-tolyl-2H-pyrazol-3-yl)-3-(2-methyl-6-piperazin-1-yl-pyridin-3-yl)-urea dihydrochloride as an off-white powder (62.2 g—contains ca. 45 mol % of dioxane. LCMS(ES+): m/z=448 [M+H].

1. concentrationthen concentrate under reduced pressure (room temperature, ca. 10 torr, 3 days)