反应 #674291

ord-21ff33de154f4f3c9b01e23b0c8d723c

反应方程式

CC(Oc1cccnc1N)c1c(Cl)ccc(F)c1Cl
3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridine-2-amine
O=C1CCC(=O)N1Br
NBS
CC(Oc1cc(Br)cnc1N)c1c(Cl)ccc(F)c1Cl
5-bromo-3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-2-amine
收率 82.5%

溶剂

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The precipitate was removed by filtration
  2. 2
    浓缩The black filtrate was concentrated
  3. 3
    其他to give a black residue which
  4. 4
    其他was purified by CombiFlash (80 g silica gel column, EtOAc/Hexane)

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09226923B2uspto-grants-2016_01