反应详情

温度

77 °C

Potassium carbonate (113 g) and deionized water (565 mL) were sequentially added to a solution of N-{7-bromo-4-[(2-hydroxy-2-methylpropyl)amino][1,5]naphthyridin-3-yl}-2-ethoxyacetamide hydrochloride (113 g, 261 mmol) in denatured ethanol (1.695 L), and the resulting mixture was heated at reflux (77° C.) overnight and allowed to cool to room temperature. The ethanol was removed under reduced pressure, and the resulting mixture was filtered to isolate a solid. The solid was washed with deionized water (100 mL) and dried over two nights in a vacuum oven at 40° C. to provide 90 g of 1-[7-bromo-2-(ethoxymethyl)-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl]-2-methylpropan-2-ol as a brown solid. Material from a separate run was used in the next step.

1. temperaturethe resulting mixture was heated
2. temperatureto cool to room temperature
3. customThe ethanol was removed under reduced pressure
4. filtrationthe resulting mixture was filtered
5. customto isolate a solid
6. washThe solid was washed with deionized water (100 mL)
7. customdried over two nights in a vacuum oven at 40° C.