Hydrochloric Acid → HCID 118208676, compound

Participants

Reaction Steps

Hydrochloric acid (6N, 6.6 mL, 39.7 mmol) was added to 4-(difluoromethyl)-N-(3-(1-((2,2-dimethyl-1,3-dioxolan-4-yl)methyl)-1H-pyrazol-4-yl)-5-methylphenyl)pyrimidin-2-amine (16.5 g, 39.7 mmol) in MeOH (150 mL). The mixture heated at reflux for 2 h then cooled to RT. Water (200 mL) was added and then the pH was adjusted to 7 with NaOH (6N). The solution was seeded with crystalline product (prepared via an earlier small scale) and crystallization occurred. Additional water (150 ml) was added and the mixture was stirred for 30 min, then filtered, washed with water (2×50 mL) and dried for 14 h under a nitrogen bag to afford 3-(4-(3-((4-(difluoromethyl)pyrimidin-2-yl)amino)-5-methylphenyl)-1H-pyrazol-1-yl)propane-1,2-diol an off white solid.

Provenance & Evidence