反应详情

A solution of methanesulfonamide (40 mg, 0.44 mmol) and DMF (0.5 ml) was added to a suspension of sodium hydride (95%) (11 mg, 0.44 mmol) and DMF (0.5 ml) under nitrogen. The mixture was stirred for 20 minutes at room temperature. A solution of methyl 2-chloro-6-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)pyrimidine-4-carboxylate (Example 6, 47 mg, 0.11 mmol) in DMF (1 ml) was added dropwise to the mixture over 5 minutes. The mixture was stirred for 1 h at room temperature and for 3 h at 60° C. The mixture was cooled to room temperature and concentrated under reduced pressure. The crude residue was purified by preparative reversed-phase HPLC (water/acetonitrile gradient, 10-90%) to afford the title compound (14 mg).

1. stirringThe mixture was stirred for 1 h at room temperature and for 3 h at 60° C
2. temperatureThe mixture was cooled to room temperature
3. concentrationconcentrated under reduced pressure
4. customThe crude residue was purified by preparative reversed-phase HPLC (water/acetonitrile gradient, 10-90%)