反応 #6429

反応方程式

hydrochloric acid

hydrochloric acid

sodium sulphite

potassium

2,3-difluorophenol

→

2,3-difluorohydroquinone

溶媒

toluene

sodium hydroxide

反応条件

後処理

1. 1
   workup.ADDITIONDuring this addition
2. 2
   抽出is extracted with ether
3. 3
   温度refluxed for 20 minutes
4. 4
   温度After cooling
5. 5
   その他the toluene layer is separated off
6. 6
   抽出the aqueous phase is extracted with ether in a perforator

実験手順

1 mol of 2,3-difluorophenol is dissolved in 1 l of 10% sodium hydroxide solution, and a saturated aqueous solution of 1.1 mol of potassium peroxodisulphate is added dropwise over the course of 4 hours with ice cooling. During this addition, the temperature must not exceed 20o The mixture is stirred overnight at room temperature and neutralized using hydrochloric acid, and unreacted starting material is extracted with ether. 3 1 of toluene and 2 mol of sodium sulphite are added to the aqueous phase, and the mixture is strongly acidified using 1 1 of concentrated hydrochloric acid and refluxed for 20 minutes. After cooling, the toluene layer is separated off, the aqueous phase is extracted with ether in a perforator, and 2,3-difluorohydroquinone is obtained by evaporating the combined toluene and ether extracts.

出典