反应详情

温度

100 °C

Degassed toluene (6 ml) and EtOH (3 ml) were added in one portion to a mixture of 4-bromo-2-isopropyl-7-(2-methylsulfanyl-ethoxy)-2H-phthalazin-1-one (0.3 g, 0.8 mmol), sodium t-butoxide (0.112 g, 1.2 mmol), 3-amino-5-methyl pyrazole (0.107 g, 1.2 mmol), tris-(dibenzylideneacetone)-dipalladium (0.038 g, 0.042 mmol) and 2-(di-t-butylphosphino)-biphenyl (0.025 g, 0.084 mmol) under nitrogen. The reaction mixture was heated to 100° C. for 20 hours with stirring and then cooled to RT. Diethyl ether (10 ml) was added and the precipitated solid was filtered to give the crude product as a grey solid. Flash column chromatography (elution: 95% EtOAc, 5% MeOH) afforded the title compound as a white solid (0.070 g, 7% yield).

1. customDegassed toluene (6 ml) and EtOH (3 ml)
2. temperaturecooled to RT
3. filtrationthe precipitated solid was filtered
4. customto give the crude product as a grey solid
5. washFlash column chromatography (elution: 95% EtOAc, 5% MeOH)