1,3-Propanediamine, N1,N1,N3-trimethyl- → Ammonium Hydroxide

Participants

Reaction Steps

3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-N,4-dimethylbenzamide, (0.02 g, 0.041 mmol) was dissolved in THF (5 mL) and [3-(dimethylamino)propyl]methylamine (0.024 g, 0.205 mmol) was added. The reaction mixture was stirred at room temperature for 6 days, but the reaction had not gone to completion. The reaction was heated to 45° C. overnight and then cooled to room temperature. The solvents were pumped off in vacuo, and the residue was flash chromatographed on silica gel (10 g) eluted with CH2Cl2 to 6:0.5:0.05, CH2Cl2:ethanol:NH4OH to give the title compound as a white amorphous solid. mp 163-165° C. LC-MS m/z 524.6 (M+H)+, 1.47 min (ret time).

Provenance & Evidence