Reaktion #546996

Reaktionsgleichung

3,4-difluorobromobenzene

piperazine

sodium tert-butoxide

BINAP

→

1-(3,4-Difluorophenyl)piperazine

Lösungsmittel

Ethyl acetate

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux overnight
2. 2
   Waschenthe mixture is then washed with water
3. 3
   Extraktionthe organic phase is extracted with 1N hydrochloric acid
4. 4
   WaschenThe aqueous phase is then washed with ethyl acetate
5. 5
   ExtraktionUsing dichloromethane, the product is extracted from the aqueous phase
6. 6
   TrocknenThe extract is then dried over magnesium sulphate
7. 7
   Sonstigethe solvent is removed
8. 8
   Sonstigethe target compound is dried under reduced pressure

Vorschrift

In 100 ml of toluene, 5 g (25.91 mmol) of 3,4-difluorobromobenzene, 13.39 g (155.45 mmol) of piperazine, 3.49 g (36.27 mmol) of sodium tert-butoxide, 0.24 g (0.26 mmol) of tris(dibenzylidene-acetone)dipalladium and 0.48 g (0.78 mmol) of BINAP are stirred under reflux overnight. Ethyl acetate is added, the mixture is then washed with water and the organic phase is extracted with 1N hydrochloric acid. The aqueous phase is then washed with ethyl acetate and subsequently adjusted to pH 8. Using dichloromethane, the product is extracted from the aqueous phase. The extract is then dried over magnesium sulphate, the solvent is removed and the target compound is dried under reduced pressure.

Quelle