反应详情

At 80° C., 98 mg (0.14 mmol) of the compound of Example 49A were stirred in 0.56 ml of trifluoroacetic acid for 3 h. The reaction was then concentrated, the residue was dissolved in ethyl acetate and the solution was washed with saturated sodium bicarbonate solution. The organic phase was dried over sodium sulphate, filtered and concentrated under reduced pressure. After drying of the residue under high vacuum, the crude product was purified by preparative HPLC (Method 29). The product fractions were combined and concentrated, and the residue was taken up in ethyl acetate and washed with saturated sodium bicarbonate solution. The organic phase was dried over sodium sulphate, filtered and concentrated under reduced pressure. Drying under high vacuum gave a first product fraction (39 mg). A second product fraction of a further 19 mg was obtained from the combined mixed fractions of the HPLC separation by concentrating these fractions followed by re-purification by the same method by preparative HPLC. This gave a total of 58 mg (69% of theory) of the title compound.

1. concentrationThe reaction was then concentrated
2. dissolutionthe residue was dissolved in ethyl acetate
3. washthe solution was washed with saturated sodium bicarbonate solution
4. dry with materialThe organic phase was dried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customAfter drying of the residue under high vacuum
8. customthe crude product was purified by preparative HPLC (Method 29)
9. concentrationconcentrated
10. washwashed with saturated sodium bicarbonate solution
11. dry with materialThe organic phase was dried over sodium sulphate
12. filtrationfiltered
13. concentrationconcentrated under reduced pressure
14. customDrying under high vacuum
15. customgave a first product fraction (39 mg)
16. customA second product fraction of a further 19 mg was obtained from the
17. additioncombined mixed
18. customfractions of the HPLC separation
19. concentrationby concentrating these fractions
20. customfollowed by re-purification by the same method by preparative HPLC