1,4-Dioxane hydrochloride → HCID 24999762, compound

Participants

Reaction Steps

To a room temperature solution of example 12, di-tert-butyl 3-(3-tert-butyl-5-{[(2-fluoro-4-{[2-(methylcarbamoyl)pyridin-4-yl]oxy}phenyl)carbamoyl]amino}-1H-pyrazol-1-yl)benzyl phosphate, (0.45 g, 0.62 mmol) in dioxane (12 mL) was slowly added HCl/dioxane (4M, 4 mL, 16 mmol). A white precipitate formed and the suspension was stirred at room temperature for 3 h. The reaction mixture was diluted with ether (20 mL) and the solids were collected. The resulting solids were washed with ether followed by hexanes to afford 0.40 g (94%) of the desired product as a white powder. MS m/z 612.9 (M+H)+; Retention time (LC-MS): 3.05 min.

Provenance & Evidence