反应详情

温度

70 °C

The product from Example 60F (0.097 g, 0.211 mmol) and 4 M hydrogen chloride in dioxane (5 mL, 20.00 mmol) were combined and heated at 70° C. for 18 hours, cooled and concentrated. The residue was partitioned between ethyl acetate and water adjusting the pH to 7. The organic layer was washed with saturated aqueous sodium chloride, dried (anhydrous Na2SO4), treated with 3-mercaptopropyl functionalized silica gel, filtered, and concentrated. Purification by trituration (1:1 dichloromethane/heptane) afforded the title compound (0.077 g, 82%). 1H NMR (300 MHz, DMSO-d6) δ ppm 11.03 (d, J=5.43 Hz, 1H) 8.02 (d, J=2.37 Hz, 1H) 7.95 (d, J=2.37 Hz, 1H) 7.75 (s, 1H) 7.39-7.50 (m, 2H) 7.10-7.19 (m, 1H) 6.93-6.97 (m, 1H) 6.66 (d, J=6.44 Hz, 1H) 4.57 (s, 2H) 4.14 (s, 3H) 2.98 (s, 3H). MS (ESI+) m/z 446 (M+H)+.

1. temperaturecooled
2. concentrationconcentrated
3. customThe residue was partitioned between ethyl acetate and water adjusting the pH to 7
4. washThe organic layer was washed with saturated aqueous sodium chloride
5. dry with materialdried (anhydrous Na2SO4)
6. additiontreated with 3-mercaptopropyl functionalized silica gel
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification by trituration (1:1 dichloromethane/heptane)