Sodium Iodide → HCID 67152470, compound

Participants

Reaction Steps

Under N2 atmosphere, to a solution of cyanoacetic acid ethyl ester (93 mg) in THF (3 mL) was added sodium hydride (33 mg) and the mixture was stirred for 30 minutes. Methanesulfonic acid 2-{1-[7-(4-bromo-2,6-dimethyl-phenyl)-2,5,6-trimethyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-piperidin-4-yl}-ethyl ester (300 mg) was added, and the mixture was heated at reflux for 3 hours. Cyanoacetic acid ethyl ester (93 mg) was added, and the reaction mixture was heated at reflux for 1 hour. And then NaI (7 mg) was added, and the mixture was heated at reflux for 2 hours. After cooling to room temperature, 5% aqueous KHSO4 solution was added into the reaction mixture and the mixture was extracted with ethyl acetate. The organic phase was dried over MgSO4 and filtered and the filtrate was concentrated under reduced pressure. The residue was purified with column chromatography (silica gel: Wako gel C200, eluent: hexane:ethyl acetate=4/1) to obtain the title compound (57 mg) as a colorless oil.

Provenance & Evidence