反应详情

温度

80 °C

7-Nitro-2-isopropyl-4-bromo-2H-phthalazin-1-one (4.6 g, 0.015 mol) was dissolved in a 5:1 mixture of EtOH and water (150 ml). To this solution was added iron powder (2.14 g, 0.039 mol) and concentrated HCl (1 ml), the mixture was heated to 80° C. for 3 hours. After this time, the reaction mixture was cooled to RT and filtered through a pad of celite, the celite was washed with EtOH (100 ml), and the solution was concentrated under vacuum to give the title compound (4.2 g, 98% yield) as a white solid. δH (400 MHz, DMSO), 7.56 (1H, d), 7.28 (1H, s), 7.13 (1 H, d), 6.47 (2H, s), 5.24-5.09 (1H, m), 1.23 (6H, d) Tr=1.34 min m/z (ES+) (M+H)+ 282, 284

1. temperatureAfter this time, the reaction mixture was cooled to RT
2. filtrationfiltered through a pad of celite
3. washthe celite was washed with EtOH (100 ml)
4. concentrationthe solution was concentrated under vacuum