Isopropanol → HCID 11949764, compound

Participants

Reaction Conditions

Reaction Steps

Dry iso-propanol (2 mL) was treated with NaH (0.00612 g, 0.153 mmol, 60% in mineral oil) under argon and stirred for 10 min. The product of Example 23d, N-{3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methylphenyl}-3-fluoro-4-methylbenzamide (0.070 g, 0.120 mmol) was added in iso-propanol (2 mL). The reaction was stirred under argon for 1 hour and then warmed to 80° C. for 3 hours. The reaction mixture was diluted with EtOAc and the organics washed with water, brine (twice), dried over Na2SO4, filtered and evaporated. The crude residue was purified by flash chromatography on silica gel, eluting with a CH2Cl2 −10% EtOAc/CH2Cl2 gradient to afford the title compound as a white solid. mp 253.5-255.4° C.; LC-MS m/z 562 (M+H)+, 2.44 min (ret. time).

Provenance & Evidence