反应详情

温度

90 °C

N-(1-chloroisoquinolin-5-yl)-N′-[4-(trifluoromethyl)benzyl]urea (Example 69; 47 mg, 0.12 mmol) was added to a mixture of 3N HCl (aq. 5 ml) and THF (1 ml). The mixture was heated at 90° C. for 20 hours, then 5N HCl (aq. 2 ml) was added and the reaction heated at 90° C. for a further 20 hours. After cooling to room temperature, ethyl acetate (20 ml) was added and the layers separated (some solid was suspended in the organic layer). The organic phase was washed with saturated aqueous NaHCO3 (20 ml), then evaporated. The residue was triturated in refluxing isopropyl alcohol (5 ml), then cooled to room temperature. The white solid was collected by filtration and washed with isopropyl alcohol (2×1 ml) to give the title compound (22 mg). m/z (ES+) 362 (M+H)+.

1. temperaturethe reaction heated at 90° C. for a further 20 hours
2. temperatureAfter cooling to room temperature
3. customthe layers separated (some solid
4. washThe organic phase was washed with saturated aqueous NaHCO3 (20 ml)
5. customevaporated
6. customThe residue was triturated
7. temperaturein refluxing isopropyl alcohol (5 ml)
8. temperaturecooled to room temperature
9. filtrationThe white solid was collected by filtration
10. washwashed with isopropyl alcohol (2×1 ml)