反应详情

LiOH.H2O (17.3 mg, 0.413 mmol) was added to a solution of tert-butyl 4-(4-((4-(2-(1-methoxy-1-oxopropan-2-yl)phenethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)piperidine-1-carboxylate (I53) (0.084 g, 0.137 mmol) in THF (7 mL), water (1.5 mL) and methanol (1 mL). The resulting mixture was allowed to stir at room temperature for 20 hours. The volatiles were removed in vacuo and the residue diluted with EtOAc (50 mL) and sat. aq. NaHCO3 (50 mL). The layers were separated and the aqueous layer was extracted with EtOAc (1×50 mL). The organic layers were combined, washed with brine (50 mL), dried with Na2SO4, filtered and concentrated under reduced pressure to give the title compound (I54) (86 mg) as a pale yellow viscous oil.

1. customThe volatiles were removed in vacuo
2. additionthe residue diluted with EtOAc (50 mL) and sat. aq. NaHCO3 (50 mL)
3. customThe layers were separated
4. extractionthe aqueous layer was extracted with EtOAc (1×50 mL)
5. washwashed with brine (50 mL)
6. dry with materialdried with Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure