反应详情

温度

90 °C

2-Fluoro-5-[(4-oxo-3,4-dihydrophthalazin-1-yl)methyl]benzonitrile (ED) (9.60 g, 34.37 mmol) and water (40 ml) were stirred at 20° C. 2M Sodium hydroxide (36 ml, 72.00 mmol) was added, the reaction mixture warmed to 90° C. and held at this temperature overnight. The reaction mixture was cooled to room temperature and filtered. The filter pad was washed with water (10 ml) and the combined filtrate added to 2M HCl (56 ml, 112.00 mmol) at 60° C. over 40 minutes. The resulting suspension was cooled to 50° C. and filtered, washed with water (57 ml) and dried in vacuo at up to 60° C. to give the title compound as a white solid (9.72 g).

1. customheld at this temperature overnight
2. temperatureThe reaction mixture was cooled to room temperature
3. filtrationfiltered
4. washThe filter pad was washed with water (10 ml)
5. temperatureThe resulting suspension was cooled to 50° C.
6. filtrationfiltered
7. washwashed with water (57 ml)
8. customdried in vacuo at up to 60° C.