反应详情

A 25 ml round-bottom flask is charged with 1-{4-[(2R,4S)-4-((3,5-bis-trifluoromethyl-benzyl)-{5-[1-(tetrahydro-pyran-2-yl)-1H-pyrazol-4-yl]-pyrimidin-2-yl}-amino)-2-ethyl-pyrrolidin-1-yl]-5-chloro-pyrimidin-2-yl}-piperidin-4-ol (0.15 mmol), 1N HCl (0.8 ml, 0.8 mmol) and MeOH (2 ml). The mixture is then heated to 60 degree for 30 minutes. After cooling down to rt, sat. NaHCO3 and dichloromethane are added, then organic layer is collected. Removal of solvent and purification with reverse phase column chromatography give 1-[4-((2R,4S)-4-{(3,5-Bis-trifluoromethyl-benzyl)-[5-(1H-pyrazol-4-yl)-pyrimidin-2-yl]-amino}-2-ethyl-pyrrolidin-1-yl)-5-chloro-pyrimidin-2-yl]-piperidin-4-ol (11.3 mg, 0.015 mmol, 10% for 2 steps).

1. temperatureThe mixture is then heated to 60 degree for 30 minutes
2. customorganic layer is collected
3. customRemoval of solvent and purification with reverse phase column chromatography