反応 #2171035

反応方程式

2,6-difluoroaniline

bromine

→

4-bromo-2,6-difluoroaniline

収率 91.7%

溶媒

acetic acid

acetic acid

反応条件

後処理

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

実験手順

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%.

出典