1-Acetylpiperazine → 1-[4-(4-Methoxy-3-nitro-phenyl)-piperazin-1-yl]ethanone

温度

100 °C

4-bromo-1-methoxy-2-nitrobenzene (30 g, 129.29 mmol), 1-(piperazin-1-yl)ethanone (16.57 g, 129.29 mmol), cesium carbonate (84 g, 258.59 mmol),diacetoxypalladium (2.322 g, 10.34 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (8.98 g, 15.52 mmol) in dioxane (200 mL) were degazed with nitrogen and stirred at 100°C for 1 hour. The reaction mixture was allowed to cool to room temperature, water (1000mL) was added and mixture was filtered on celite. The aq. layer was extracted with CH2Cl2 (2X500mL). The organic layer was dried on MgSO4, filtered and concentrated to dryness to afford the crude product. This product was purified by flash chromatography on silica gel eluting with ethyl acetate - methanol (92-8), the solvents were evaporated to dryness to afford 1-(4-(4-methoxy-3-nitrophenyl)piperazin-1-yl)ethanone (10.80 g, 29.9 %)

ORDレコード

ord-8b6e9d49ac804667b43344fcaf4ab862

出典データセット

750 AstraZeneca ELN dataset

元リンク

出典を表示