反应详情

TFA (0.50 mL, 6.5 mmol) was added to a mixture of tert-Butyl 4-(5-((4-(2-(1-carbamoylcyclopropyl)phenethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)pyridin-2-yl)piperidine-1-carboxylate A79 (0.080 g, 0.13 mmol) in DCM (5 mL) and the mixture stirred for 4 hours. The mixture was concentrated under reduced pressure and quenched with 25% aqueous NaOH (20 mL) before extracting with EtOAc (3×20 mL). The combined organic extracts were concentrated under reduced pressure and the above procedure repeated with DCM (1.5 mL) and TFA (0.2 mL) for 3 hours. The mixture was concentrated under reduced pressure and quenched with 25% aqueous NaOH (20 mL) before extracting with EtOAc (3×20 mL). The combined organic residues were dried (phase separation cartridge) and concentrated under reduced pressure to give the title compound 68 (0.069 g, quantitative). LCMS-A: rt 4.783 min; m/z 511.3 [M+H]+.

1. concentrationThe mixture was concentrated under reduced pressure
2. customquenched with 25% aqueous NaOH (20 mL)
3. extractionbefore extracting with EtOAc (3×20 mL)
4. concentrationThe combined organic extracts were concentrated under reduced pressure
5. waitthe above procedure repeated with DCM (1.5 mL) and TFA (0.2 mL) for 3 hours
6. concentrationThe mixture was concentrated under reduced pressure
7. customquenched with 25% aqueous NaOH (20 mL)
8. extractionbefore extracting with EtOAc (3×20 mL)
9. customThe combined organic residues were dried
10. custom(phase separation cartridge)
11. concentrationconcentrated under reduced pressure