反应详情

温度

0 °C

To a solution of tert-Butyl 4-(4-carbamoyl-3-{[4-(2-methoxy-2-oxoethyl)phenyl]amino}-1H-pyrazol-1-yl)-4-(cyanomethyl)piperidine-1-carboxylate (226 mg, 0.46 mmol) in THF (2.3 mL) at 0° C. was added KOtBu (0.68 mL, 0.68 mmol, 1.0M in THF), and the mixture was stirred at 0° C. for 20 minutes, then ambient temperature for 20 minutes. The mixture was diluted with saturated aqueous NH4Cl, and extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous MgSO4, and concentrated in vacuo. Et2O (5 mL) was added to the resulting oily residue and a solid precipitated out. This solid was collected by decant, and washed with Et2O to afford the title compound. LRMS (ESI) calc'd for C13H15N4O3 [M+H]+: 275. Found: 275.

1. waitambient temperature for 20 minutes
2. extractionextracted with EtOAc
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous MgSO4
5. concentrationconcentrated in vacuo
6. additionEt2O (5 mL) was added to the resulting oily residue
7. customa solid precipitated out
8. customThis solid was collected
9. customby decant
10. washwashed with Et2O