反应详情

温度

75 °C

1.0N isopropyl sulfuric acid (0.19 mL, 1.04 eq) in IPA was added to a solution of (S)-2-amino-3-(4-(2-amino-6-((R)-1-(4-chloro-2-(3-methyl-1H-pyrazol-1-yl)phenyl)-2,2,2-trifluoroethoxy)pyrimidin-4-yl)phenyl)propanoic acid free base (3.66 mL, 0.05M, 0.183 mmol) in MeOH and followed by evaporation of solvent to dry. After adding of 6.5 mL MeCN/IPA (3/1) and heating at 75° C., a clear solution was obtained. 2.0 mL solvent was evaporated and stirred overnight. The precipitate was collected by filtration. The cake was washed with heptane, dried at 45° C. under vacuum overnight to give 68 mg (S)-2-amino-3-(4-(2-amino-6-((R)-1-(4-chloro-2-(3-methyl-1H-pyrazol-1-yl)phenyl)-2,2,2-trifluoroethoxy)pyrimidin-4-yl)phenyl)propanoic acid isopropyl sulfate, (54% yield).

1. customfollowed by evaporation of solvent
2. customto dry
3. additionAfter adding of 6.5 mL MeCN/IPA (3/1)
4. customa clear solution was obtained
5. custom2.0 mL solvent was evaporated
6. filtrationThe precipitate was collected by filtration
7. washThe cake was washed with heptane
8. customdried at 45° C. under vacuum overnight