反应详情

温度

80 °C

Palladium (II) acetate (36 mg, 0.16 mmol) was added to a suspension of 3-chloro-1-(4-fluoro-phenyl)-1H-pyrazin-2-one (0.71 g, 3.2 mmol), phenoxyacetamide (0.57 g, 3.8 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (0.138 g, 0.24 mmol) and Cs2CO3 (1.5 g, 4.45 mmol) in 1,4-dioxane (10 mL). The mixture was stirred at 80° C. for 15 minutes. Then DCM was added, the solid was filtered off and washed with more DCM. The filtrate was separated and the solvent evaporated in vacuo and the crude product was purified by flash column chromatography (silica; AcOEt in DCM 1/99 to 1/4). The desired fractions were collected and the solvents evaporated in vacuo to yield N-[4-(4-fluoro-phenyl)-3-oxo-3,4-dihydro-pyrazin-2-yl]-2-phenoxy-acetamide (0.38 g, 84% yield).

1. filtrationthe solid was filtered off
2. washwashed with more DCM
3. customThe filtrate was separated
4. customthe solvent evaporated in vacuo
5. customthe crude product was purified by flash column chromatography (silica; AcOEt in DCM 1/99 to 1/4)
6. customThe desired fractions were collected
7. customthe solvents evaporated in vacuo