反应详情

To a solution of 5-chloro-N2-(1,3-dimethyl-1H-pyrazol-4-yl)-N4-(octahydrocyclopenta[c]pyrrol-5-yl)pyrimidine-2,4-diamine (186.6 mg, 0.54 mmol) and 2-cyanoacetic acid (64.8 mg, 0.76 mmol) in a mixture of DCM (20 mL) and DMF (5 mL) were added HATU (374.3 mg, 0.98 mmol) and Et3N (151.8 mg, 1.50 mmol). After addition, the reaction mixture was stirred at rt for 1 h, quenched with H2O (30 mL) and extracted with DCM (100 mL×3). The combined organic phases were washed with brine (100 mL), dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (MeOH/DCM (v/v)=1/50) to give the title compound as a beige solid (124.5 mg, 55.9%).

1. additionAfter addition
2. customquenched with H2O (30 mL)
3. extractionextracted with DCM (100 mL×3)
4. washThe combined organic phases were washed with brine (100 mL)
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue was purified by silica gel column chromatography (MeOH/DCM (v/v)=1/50)