Dimethyl malonate → HCID 86642125, compound

Participants

Reaction Steps

To a solution of dimethyl malonate (0.39 mL, 3.37 mmol) in THF (20 mL) was added sodium hydride (60% dispersion in oil, 138 mg, 3.37 mmol) portionwise. The reaction mixture was stirred for 10 minutes at r.t. then 4,6-dichloro-2-methylpyrimidine (500 mg, 3.07 mmol) was added and the mixture heated to reflux for 2 h. The resulting suspension was concentrated in vacuo, triturated with Et2O (3×30 mL) and the mother liquors were evaporated in vacuo to yield the title compound (300 mg, 40%) as an off-white solid. LCMS (ES+) 259.0 (M+H)+, RT 2.93 minutes (90% purity) (Method 2).

Provenance & Evidence