反应详情

温度

50 °C

To a suspension of 5-(2-acetamido-5-methylpyridin-4-yl)-2-bromo-3-furamide (8.5 g, 25.2 mmol) in dry toluene (260 mL) was added DMF-DMA (8.85 g, 74.0 mmol). The reaction mixture was allowed to stir at 50° C. overnight and then concentrated. The residue was resuspended in AcOH (90 mL) and hydrazine (3.77 g, 117.6 mmol) was added dropwise at rt. The reaction mixture was allowed to stir for 2 h and then concentrated. The mixture was azeotroped several times with toluene and then the residue was suspended in EtOAc and water. The mixture was basified with saturated aqueous NaHCO3 to pH=8.5. The mixture was filtered and the solid was dried to give N-{4-[5-bromo-4-(1H-1,2,4-triazol-3-yl)-2-furyl]-5-methylpyridin-2-yl}acetamide (6.0 g, 66%).

1. concentrationconcentrated
2. stirringto stir for 2 h
3. concentrationconcentrated
4. customThe mixture was azeotroped several times with toluene
5. filtrationThe mixture was filtered
6. customthe solid was dried