反应详情

温度

100 °C

5-((7-bromo-4-oxo-3,4-dihydrophthalazin-1-yl)methyl)-2-fluorobenzonitrile (96) (2.4 g, 6.70 mmol) and potassium hydroxide (3.76 g, 67.01 mmol) were added to ethanol (20 mL) and water (80 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, which was filtered, washed with water and dried to the desired material as a beige solid. (2.000 g, 79% yield); 1H NMR (400.132 MHz, DMSO) δ 4.37 (2H, s), 7.26 (1H, t), 7.61-7.57 (1H, m), 7.83-7.82 (1H, m), 8.01 (1H, d), 8.18 (1H, d), 8.22 (1H, s), 12.67 (1H, s), 13.19 (1H, s); m/z (LC-MS, ESI+), RT=0.88 (M+H 376).

1. customThe ethanol was evaporated off
2. extractionthe aqueous was extracted with ethyl acetate (1×75 mL)
3. customto afford a solid, which
4. filtrationwas filtered
5. washwashed with water
6. dry with materialdried to the desired material as a beige solid
7. customm/z (LC-MS, ESI+), RT=0.88 (M+H 376)