Piperazine → HCID 22124974, compound

Participants

Reaction Steps

A solution of 58 mg (0.1 mmol) of 7-anilino-3-(2,4-dichlorophenyl)-3,4-dihydro-1-[3-(2-methanesulfonyloxyethyl)phenyl]-pyrimido[4,5-d]pyrimidin-2(1H)-one (prepared in Example 74) and 100 mg of piperazine in 2 ml of ethanol was heated at 50° C. for 3 hours. The reaction mixture was evaporated and the crude material purified by flash chromatography on silica gel, eluting with dichloromethane/methanol/acetic acid/water (90:18:3:2). Product containing fractions were combined and evaporated. The residue was dissolved in 10 ml of dichloromethane, washed with saturated aqueous sodium bicarbonate (10 ml), dried over magnesium sulfate, filtered and evaporated to give 3 mg (5%) of 7-anilino-3-(2,4-dichlorophenyl)-3,4-dihydro-1-[3-[2-(1-piperazinyl)-ethyl]phenyl]-pyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid of melting point 126° C. [Mass spectrum (ESI) MH+ =574].

Provenance & Evidence