Reaktion #361346

Reaktionsgleichung

chlorodifluoromethane

4-iodophenol

sodium hydroxide

THF

→

1-Difluoromethoxy-4-iodobenzene

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe mixture is evaporated in a rotary evaporator
2. 2
   workup.ADDITIONafter the addition of 200 ml of toluene
3. 3
   workup.STIRRINGthe mixture is then stirred for 1 hour
4. 4
   workup.STIRRINGIt is then stirred at about +5° C. for 18 hours
5. 5
   SonstigeThe solution above the resulting slurry-like precipitate was decanted off
6. 6
   SonstigeIt was evaporated in a rotary evaporator
7. 7
   Sonstigethe residue was chromatographed through a silica gel column

Vorschrift

100 g (0.455 mol) of 4-iodophenol and 54.6 g (1.365 mol) of sodium hydroxide are added to a mixture of 300 ml of THF and 30 ml of water. After stirring for about 1/2 hour, the mixture is evaporated in a rotary evaporator; this is repeated after the addition of 200 ml of toluene. The residue is taken up in 400 ml of THF. The mixture is cooled to 0° C., 47.1 g (0.545 mol) of chlorodifluoromethane are introduced, and the mixture is then stirred for 1 hour. It is then stirred at about +5° C. for 18 hours. The solution above the resulting slurry-like precipitate was decanted off. It was evaporated in a rotary evaporator, and the residue was chromatographed through a silica gel column, using petroleum ether as eluent.

Quelle