反应详情

温度

60 °C

To a solution of methyl 4-(1-(5-chloro-2-(3-((2,4-difluorophenyl)amino)azetidin-1-yl)nicotinamido)cyclopropyl)benzoate (D169) (12 mg, 0.024 mmol) in a mixture 1-4 dioxane/water (3 ml/1 ml), 1N NaOH (0.036 ml) was added. The reaction mixture was stirred 12 h at 60° C. Organic solvent was evaporated in vacuo and the reaction mixture was acidified with 2N HCl (pH=2) and the resulting mixture was extracted with ethylacetate (3×5 ml). Combined organics were evaporated in vacuo and the residue was loaded on SNAP-C18 gold cartridge (15 g) eluting with H2O-AcOH (0.1%)/CH3CN—AcOH (0.1%) from 10/90 to 0/100. Collected fractions were evaporated in vacuo to afford the title (E35) (5 mg)

1. customOrganic solvent was evaporated in vacuo
2. extractionthe resulting mixture was extracted with ethylacetate (3×5 ml)
3. customCombined organics were evaporated in vacuo
4. washeluting with H2O-AcOH (0.1%)/CH3CN—AcOH (0.1%) from 10/90 to 0/100
5. customCollected fractions were evaporated in vacuo