反应详情

Et3N (0.5 mL) was added to 2-(2-((2-((1H-pyrazol-4-yl)amino)-5-(trifluoromethyl)pyrimidin-4-yl)ethynyl)phenyl)propanamide A63 (0.211 g, 0.527 mmol) and 10% Pd/C (0.155 g) in DMF (4 mL) and EtOAc (16 mL) and the mixture was stirred under a hydrogen atmosphere for 16 hours. The mixture was filtered through Celite, concentrated under reduced pressure and purified using silica gel column chromatography (80-100% EtOAc in petroleum benzine 40-60° C. then 0-10% MeOH in EtOAc). The resulting product was further triturated with a mixture of Et2O and acetone and the precipitate was collected by vacuum filtration to give the title compound 54 (0.055 g, 26%). LCMS-D: rt 3.178 min; m/z 405.2 [M+H]+.

1. filtrationThe mixture was filtered through Celite
2. concentrationconcentrated under reduced pressure
3. custompurified
4. custom80-100% EtOAc in petroleum benzine 40-60° C.
5. customThe resulting product was further triturated with a mixture of Et2O and acetone
6. filtrationthe precipitate was collected by vacuum filtration