反应详情

LiOH.H2O (41 mg, 0.97 mmol) was added to a solution of tert-butyl 4-(4-((4-(2-(1-(methoxycarbonyl)cyclobutyl)phenethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)piperidine-1-carboxylate A55 (31 mg, 0.049 mmol) in THF (5 mL) and H2O (0.5 mL) and the mixture was stirred at 40° C. overnight. Additional LiOH.H2O (400 mg, 9.53 mmol) was added and the mixture was heated at reflux for 12 days. Upon cooling DCM (50 mL) and water (50 mL) were added and the aqueous layer was extracted with EtOAc (2×50 mL). The combined organics were dried (Na2SO4) and the volatiles were removed in vacuo to give the title compound A56 as a yellow oil (30 mg, 98%). LCMS-A: rt 7.586 min, m/z 625 [M+H]+.

1. temperaturethe mixture was heated
2. temperatureat reflux for 12 days
3. additionwere added
4. extractionthe aqueous layer was extracted with EtOAc (2×50 mL)
5. dry with materialThe combined organics were dried (Na2SO4)
6. customthe volatiles were removed in vacuo