N-Isopropylethylenediamine → Ammonium Hydroxide

Participants

Reaction Steps

The compound 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, (0.060 g, 0.106 mmol) was dissolved in THF (5 mL) and N-isopropylethylenediamine (0.1 g, 0.98 mmol) was added. The mixture was stirred under argon at room temperature for 3 h. The solvents were pumped off in vacuo. The residue was taken up in EtOAc washed with 1M NaOH (1×), brine (1×), dried over anhydrous Na2SO4, filtered and evaporated The residue was flash chromatographed on silica gel (10 g) eluted with 6:0.5:0.05, CH2Cl2:ethanol:NH4OH to give the title compound as a off-white amorphous solid. mp 133-137° C.; LC-MS m/z 586 (M+H)+, 1.5 min (ret. time).

Provenance & Evidence