1-Methylpiperazine → Ammonium Hydroxide

Participants

Reaction Steps

The 3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-(phenylmethyl)benzamide (0.056 g, 0.1 mmol) was dissolved in THF (5 mL) and 1-methylpiperazine (0.0303 g, 0.3 mmol) was added. The reaction was stirred for 72 h. The solvents were pumped off in vacuo, and the residue taken up in EtOAc and washed with 1 N NaOH, brine, dried over anhydrous Na2SO4 filtered and evaporated. The residue was flash chromatographed on silica gel (20 g) eluted with 6:0.1:0.01 to 6:0.3:0.03, CH2Cl2:ethanol:NH4OH to give the title compound as a white amorphous solid. mp 164-168° C. LC-MS m/z 584 (M+H)+, 1.85 min (ret time).

Provenance & Evidence