Methyl iodide → HCID 86710525, compound

Participants

Reaction Steps

To a solution of 6-chloro-2-N-(6-fluoropyridin-3-yl)-1,3,5-triazine-2,4-diamine (Intermediate 159, 0.52 g, 2.17 mmol) in DMF (1 mL) at 0 C under nitrogen was added portionwise sodium hydride (60% dispersion in mineral oil, 0.0869 g, 2.17 mmol). The mixture was stirred for 5 min, then iodomethane (0.3 g, 2.17 mmol) was added and the mixture was heated to 50 C for 16 h. EtOAc was added and the organic layer was washed with saturated aq. sodium bicarbonate, dried over sodium sulfate and concentrated. The residue was purified by FCC, eluting with 10-50% EtOAc in heptane to afford the title compound (0.089 g, 16% yield). Method B HPLC-MS: MH+ requires m/z=255 Found: m/z=255, Rt=1.52 min (74%).

Provenance & Evidence