反应详情

温度

65 °C

A suspension 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, 150 mg, 0.34 mmol), 2-mercaptoethanol (31 mg, 0.40 mmol) and potassium carbonate (139 mg, 1.01 mmol) in DMF (3 ml) were stirred at 65° C. under nitrogen for 3 hours. The mixture was cooled to room temperature and diluted with EtOAc (75 ml) and 1 N HCl (3 ml). The organic layer was separated, dried over Na2SO4, filtered and concentrated under vacuum. Purification of the residue by reversed-phase HPLC (water/acetonitrile gradient, 10-95%) gave 39 mg of the title compound.

1. temperatureThe mixture was cooled to room temperature
2. customThe organic layer was separated
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customPurification of the residue by reversed-phase HPLC (water/acetonitrile gradient, 10-95%)