4-Piperidinamine → Ammonium Hydroxide

Participants

Reaction Steps

The compound N-{3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methylphenyl}-3-fluoro-4-methylbenzamide (0.080 g, 0.137 mmol) and 4-aminopiperidine (0.055 g, 0.551 mmol) were suspended in THF (3 mL) and stirred under argon for 3 days. The completed reaction mixture was diluted with EtOAc and the organic phase washed with water, brine (twice), dried over Na2SO4, filtered and concentrated. The crude residue was purified by flash chromatography on silica gel, eluting with 6:0.5:0.05 CH2Cl2:EtOH:NH4OH to afford the title compound as an off-white solid. mp 240° C.; LC-MS m/z 602 (M+H)+, 1.79 min (ret. time).

Provenance & Evidence