反应详情

A solution of tert-butyl 4-(5-((4-(2-(1-carbamoylcyclopropyl)phenethyl)-5-methylpyrimidin-2-yl)amino)pyridin-2-yl)piperidine-1-carboxylate A45 (0.200 g, 0.359 mmol) in DCM (10 mL) was treated with TFA (0.41 mL, 5.4 mmol) and stirred at room temperature for 4 hours. An extra aliquot of TFA (0.14 mL, 1.8 mmol) was added to the reaction mixture and stirring was continued for 1 hour at room temperature. Sat. aq. NaHCO3 (˜20 mL) was carefully added to the mixture followed by aq. NaOH (2 M, ˜20 mL). DCM was removed in vacuo and the aqueous mixture was extracted with EtOAc (3×30 mL). The organic extracts were combined, washed with brine, dried (MgSO4) and the solvent removed in vacuo. The residue was dissolved in DCM before cyclohexane was added to form a white precipitate. The suspension was sonicated for 10 minutes and filtered to give the title compound A46 as a white solid (0.129 g, 79%). LCMS-D: rt 3.08 min; m/z 457 [M+H]+.

1. stirringstirring
2. waitwas continued for 1 hour at room temperature
3. customDCM was removed in vacuo
4. extractionthe aqueous mixture was extracted with EtOAc (3×30 mL)
5. washwashed with brine
6. dry with materialdried (MgSO4)
7. customthe solvent removed in vacuo
8. dissolutionThe residue was dissolved in DCM before cyclohexane
9. additionwas added
10. customto form a white precipitate
11. customThe suspension was sonicated for 10 minutes
12. filtrationfiltered