反应详情

To a solution of EXAMPLE 7A (1.26 g, 5 mmol) in pyridine (10 mL) was added ethyl isocyanate (1.18 mL, 15 mmol). The solution was heated at reflux for 7 hours, cooled, concentrated and the residue triturated with methanol. The solid was collected by filtration, washed with methanol and dried to give 493 mg (35%) of the title compound. 1H NMR (DMSO-d6) 1.72-1.83 (m, 4H), 2.49-2.55 (m, 2H), 2.57 (s, 3H), 3.05 (t, J=5.2 Hz, 2H), 7.24 (t, J=7.4 Hz, 1H), 7.43-7.53 (m, 2H), 8.19 (d, J=7.7 Hz, 2H), 11.27 (br s, 1H).

1. temperatureThe solution was heated
2. temperatureat reflux for 7 hours
3. temperaturecooled
4. concentrationconcentrated
5. customthe residue triturated with methanol
6. filtrationThe solid was collected by filtration
7. washwashed with methanol
8. customdried