1,4'-Bipiperidine → 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 (0.015 g, 0.031 mmol) was dissolved in THF (5 mL) and 1,4′-bipiperidine (0.026 g, 0.155 mmol) was added. The reaction mixture was stirred at room temperature for 4 days. 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 (dec) 179-184° C. LC-MS m/z 576 (M+H)+, 1.54 min (ret time).

Provenance & Evidence