반응 #674291

반응 방정식

3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridine-2-amine

NBS

→

5-bromo-3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-2-amine

수율 82.5%

용매

CH3CN DCM

반응 조건

후처리

1. 1
   기타The precipitate was removed by filtration
2. 2
   농축The black filtrate was concentrated
3. 3
   기타to give a black residue which
4. 4
   기타was purified by CombiFlash (80 g silica gel column, EtOAc/Hexane)

실험 절차

To a solution of 3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridine-2-amine (7.49 g, 24.87 mmol) in CH3CN/DCM (100/30 mL) was added NBS (4.43 g, 24.87 mmol) in portions at 0° C. The reaction solution was stirred at 0° C. for 10 min. The precipitate was removed by filtration. The black filtrate was concentrated to give a black residue which was purified by CombiFlash (80 g silica gel column, EtOAc/Hexane) to afford 5-bromo-3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-2-amine (7.8 g, 82%) as a pale yellow solid.

출처