Hydrazine hydrate (1:1) → HCID 22125180, compound

Participants

Reaction Steps

A solution of 500 mg (0.86 mmol) of 7-anilino-3,4-dihydro-3-(2,6-dimethylphenyl)-1-[3-(2-phthalimidoethyl)phenyl]pyrimido[4,5-d]pyrimidin-2(1H)-one in 30 ml of ethanol was treated with 0.8 ml of hydrazine hydrate. After 18 hours the mixture was evaporated and the product purified by column chromatography on silica gel using dichloromethane/methanol/acetic acid/water (240:24:3:2) for the elution. Product-containing fractions were combined, evaporated and the residue evaporated with toluene. The residue was then dissolved in 50 ml of dichloromethane, washed with 50 ml of saturated aqueous sodium bicarbonate solution, dried over magnesium sulfate, filtered and evaporated. Trituration of the residue with hexane followed by filtration afforded 10 mg (3%) of 1-[3-(2-aminoethyl)phenyl]-7-anilino-3,4-dihydro-3-(2,6-dimethylphenyl)-pyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid of melting point 128° C.

Provenance & Evidence