反应详情

温度

85 °C

The compound of Example 5E (3.449 g., 9.45 mmole) was dissolved in methanol (80 mL) containing 4N HCl in dioxane (80 mL)was stirred for 16 hours. The mixture was concentrated under reduced pressure, dissolved in chloroform washed with aqueous KHCO3, dried (Na2SO4), filtered and reduced under pressure. The residue was dissolved in toluene (450 mL), toluenesulfonic acid H2O (7.18 g.) was added and the solution was heated at 85° C. for 30 minutes. The mixture was cooled, washed with aqueous KHCO3, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was purified on silica eluting with CH2Cl2 to provide the titled compound (2.49 g, 87%).

1. concentrationThe mixture was concentrated under reduced pressure
2. dissolutiondissolved in chloroform
3. washwashed with aqueous KHCO3
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. dissolutionThe residue was dissolved in toluene (450 mL)
7. additiontoluenesulfonic acid H2O (7.18 g.) was added
8. temperatureThe mixture was cooled
9. washwashed with aqueous KHCO3
10. dry with materialdried (Na2SO4)
11. filtrationfiltered
12. concentrationconcentrated under reduced pressure
13. customThe residue was purified on silica eluting with CH2Cl2