反应详情

To a solution of {3-[3-((S)-2-amino-1,4,5,5-tetramethyl-6-oxo-1,4,5,6-tetrahydro-pyrimidin-4-yl)-4-fluoro-phenylamino]-cyclopentyl}-acetic acid methyl ester (example 95, 0.05 mmol) in THF (1 ml), MeOH (0.3 ml), and H2O (0.3 ml) was added LiOH (1N, 0.1 mmol) and the reaction mixture was stirred at room temperature for 4 h. The mixture was concentrated in vacuo and the residue diluted with aqueous HCl (0.5N) until pH=5 and EtOAc. The white solid which precipitate was filtered off, washed with H2O and dried. The organic phase was dried over Na2SO4 and evaporated to yield a white solid. The combined solid material was triturated with a mixture of dichloromethane and MeOH (10:1), filtered and the filtrate was concentrated in vacuo to yield a mixture of isomers of the title compound as a white solid. MS (ESI): m/z=405.5 [M+H]+.

1. concentrationThe mixture was concentrated in vacuo
2. additionthe residue diluted with aqueous HCl (0.5N) until pH=5 and EtOAc
3. filtrationThe white solid which precipitate was filtered off
4. washwashed with H2O
5. customdried
6. dry with materialThe organic phase was dried over Na2SO4
7. customevaporated
8. customto yield a white solid
9. customThe combined solid material was triturated with a mixture of dichloromethane and MeOH (10:1)
10. filtrationfiltered
11. concentrationthe filtrate was concentrated in vacuo
12. customto yield