反应详情

温度

100 °C

5-((8-chloro-4-oxo-3,4-dihydrophthalazin-1-yl)methyl)-2-fluorobenzonitrile (102) (6.1 g, 19.44 mmol) and potassium hydroxide (10.91 g, 194.44 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 compound as a beige solid (5.73 g, 89%); 1H NMR (400.132 MHz, DMSO) δ 4.63 (2H, s), 7.21 (1H, dd), 7.44-7.40 (1H, m), 7.64 (1H, dd), 7.82 (1H, t), 7.98 (1H, dd), 8.34 (1H, dd), 12.87 (1H, s), 13.12 (1H, s); m/z (LC-MS, ESI+), RT=0.87 (M+H 333).

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