反応 #44697

反応方程式

2,6-difluorobenzonitrile

potassium carbonate

3-chloro-4-hydroxyaniline

→

2-(4-Amino-2-chlorophenoxy)-6-fluorobenzonitrile

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度the mixture is heated
2. 2
   温度at reflux for 45 min
3. 3
   ろ過The mixture is filtered
4. 4
   洗浄the filtercake is washed with ethyl acetate and DCM
5. 5
   その他The solvent is removed under reduced pressure

実験手順

1.00 g (7.19 mmol) of 2,6-difluorobenzonitrile is initially charged in 10 ml of acetonitrile. 1.99 g (14.4 mmol) of potassium carbonate and 1.03 g (7.19 mmol) of 3-chloro-4-hydroxyaniline are added, and the mixture is heated at reflux for 45 min. The mixture is filtered and the filtercake is washed with ethyl acetate and DCM. The solvent is removed under reduced pressure and the residue is by column chromatography (silica gel 60, gradient column: mobile phase: DCM:petroleum ether=2:1, then DCM).

出典