反应 #2171035

ord-cc6b385e0f6746c092e513de05a175bf

反应方程式

Nc1c(F)cccc1F
2,6-difluoroaniline
BrBr
bromine
Nc1c(F)cc(Br)cc1F
4-bromo-2,6-difluoroaniline
收率 91.7%

反应条件

温度
10°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the precipitated crystals are filtered off with suction
  2. 2
    洗涤washed a number of times with a total of 3000 ml of ice-water
  3. 3
    其他the crystals are dried over Al2O3 under reduced pressure

实验过程

507.5 g of 2,6-difluoroaniline are added to 2500 ml of acetic acid, the mixture is cooled to 10° C., and a solution of 195 ml of bromine in 250 ml of acetic acid is added dropwise at 10-15° C. over the course of 3 hours. The mixture is subsequently stirred at room temperature for a further 1 hour and poured into 5000 ml of ice-water, the precipitated crystals are filtered off with suction and washed a number of times with a total of 3000 ml of ice-water, and the crystals are dried over Al2O3 under reduced pressure, giving 4-bromo-2,6-difluoroaniline, yield 91.7%, GC 99.6%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06716491B2uspto-grants-2004_04