反应详情

A solution of intermediate INT 37 (3.4 g, 11.26 mmol) in MeOH (75 mL) was treated with HCl (4 M in dioxane, 5.63 mL, 22.53 mmol) and stirred overnight. After evaporation of the solvents, a white solid was obtained which was washed with Et2O. The solid was then dissolved in water, slightly acidified with 2 M HCl and washed with EtOAc. The aqueous layer was separated and the pH adjusted to about 11 using 2 M NaOH followed by extraction with Et2O (3×). The Et2O layers were combined, dried over sodium sulfate, filtered and concentrated.

1. customAfter evaporation of the solvents
2. customa white solid was obtained which
3. washwas washed with Et2O
4. dissolutionThe solid was then dissolved in water
5. washwashed with EtOAc
6. customThe aqueous layer was separated
7. extractionfollowed by extraction with Et2O (3×)
8. dry with materialdried over sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated