反应详情

温度

70 °C

A mixture of 4-(3,4-methylenedioxyphenyl)-6,7-methylenedioxy-1(2H)-phthalazinone (133 mg, 0.43 mmol), 1-(2-bromoethyl)imidazole hydrogen bromide (439 mg, 1.72 mmol), and K2CO3 (415 mg, 3.0 mmol) in DMF (10 mL) was stirred for 5 h at 70° C. The mixture was cooled, and 2N HCl and EtOAc were added to the mixture. The acidic aqueous layer was separated, made alkaline with 5% K2CO3 solution, and extracted with EtOAc. The extract was washed with brine, dried and concentrated under reduced pressure. The residual solid were purified by chromatography on silica gel with CHCl3-MeOH (20:1) to afford the product as a white solid (27 mg, 16%). 300 MHz 1H-NMR (CDCl3): δ 7.78 (s, 1H), 7.37 (s, 1H), 7.04-6.86 (m, 5H), 6.13 (s, 2H), 6.03 (s, 2H), 4.58 (m, 2H), 4.45 (m, 2H).

1. temperatureThe mixture was cooled
2. customThe acidic aqueous layer was separated
3. extractionextracted with EtOAc
4. washThe extract was washed with brine
5. customdried
6. concentrationconcentrated under reduced pressure
7. customThe residual solid were purified by chromatography on silica gel with CHCl3-MeOH (20:1)