反应详情

温度

80 °C

To a solution of 2-chloro-5-nitro-pyridine (450 mg, 2.84 mmol) in isopropanol (10 mL)/DMF (7 mL) was added 60% NaH (57 mg). The mixture was stirred at 80° C. for 4 h and the organic solvents were evaporated under reduced pressure. The residue was partitioned between EtOAc and water. The EtOAc extracts were dried (Na2SO4) and evaporated. The crude product was used for the next step reaction without further purification. 1H NMR (300 MHz, CDCl3) δ 9.06 (d, J=2.81 Hz, 1H), 8.32 (dd, J=8.79 and 2.53 Hz, 1H), 6.74 (d, J=8.61 Hz, 1H), 5.43 (m, 1H), 1.38 (d, J=6.20 Hz, 6H).

1. customthe organic solvents were evaporated under reduced pressure
2. customThe residue was partitioned between EtOAc and water
3. dry with materialThe EtOAc extracts were dried (Na2SO4)
4. customevaporated
5. customThe crude product was used for the next step reaction without further purification