反应详情

温度

0 °C

To a solution of 4-fluoropyridin-2-amine (400 mg, 3.57 mmol) in acetonitrile (35. 7 mL) was added NBS (648 mg, 3.64 mmol) in three portions at 0° C. The reaction mixture was stirred at 0° C. for 20 min. LCMS showed the reaction complete. After quenched with sat Na2S2O3 and NaHCO3, stirred for 30 min. The reaction mixture was extracted with EtOAc 3 times. Washed by sat NaHCO3, water and brine. Dried and concentrated. The crude material was triturated with ether and taken to the next step without further purification. LCMS (m/z): 192.9 (MH+), 0.32 min.

1. customthe reaction complete
2. customAfter quenched with sat Na2S2O3 and NaHCO3
3. stirringstirred for 30 min
4. extractionThe reaction mixture was extracted with EtOAc 3 times
5. washWashed
6. customDried
7. concentrationconcentrated
8. customThe crude material was triturated with ether
9. customtaken to the next step without further purification
10. custom192.9 (MH+), 0.32 min.