反应详情

温度

100 °C

3-((8-chloro-4-oxo-3,4-dihydrophthalazin-1-yl)methyl)benzonitrile (117) (3.75 g, 12.68 mmol) and potassium hydroxide (7.11 g, 126.81 mmol) were added to ethanol (30 mL) and water (70 mL) and heated at 100° C. for 5 hours. The ethanol was evaporated off and the aqueous was extracted with ethyl acetate (1×75 mL). The aqueous was then acidified to pH1 with conc HCl to afford a solid, this was filtered, washed with water and dried to afford the desired material as a beige solid (3.81 g, 95% yield); 1H NMR (400.132 MHz, DMSO) δ 4.67 (2H, s), 7.42-7.41 (2H, m), 7.72 (1H, s), 7.79-7.76 (1H, m), 7.81 (1H, t), 7.97 (1H, dd), 8.34 (1H, dd), 12.88 (1H, s); m/z (LC-MS, ESI+), RT=0.92 (M+H 315).

1. customThe ethanol was evaporated off
2. extractionthe aqueous was extracted with ethyl acetate (1×75 mL)
3. customto afford a solid
4. filtrationthis was filtered
5. washwashed with water
6. customdried