Reaktion #49733

Reaktionsgleichung

Thiophenol

2-nitro-4-trifluoromethylbenzonitrile

thiophenol

potassium carbonate

Water

→

2-(phenylsulphenyl)-4-trifluoromethylbenzonitrile

Ausbeute 85.2%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthen heated
2. 2
   Temperaturat reflux for 9 hours
3. 3
   workup.STIRRINGthe mixture was stirred
4. 4
   Temperaturheated
5. 5
   Temperaturat reflux for 1 hour
6. 6
   Extraktionthe mixture was extracted with dichloromethane
7. 7
   Trocknendried (MgSO4)
8. 8
   Filtrationfiltered
9. 9
   SonstigeThe flitrate was evaporated to dryness
10. 10
    Sonstigethe residue was recrystallized from n-hexane

Vorschrift

A mixture of 2-nitro-4-trifluoromethylbenzonitrile (8.64 g), thiophenol (4.4 g) and potassium carbonate (6.9 g) in acetonitrile was stirred at room temperature for 1 hour then heated at reflux for 9 hours. Thiophenol (0.3 ml) was added and the mixture was stirred and heated at reflux for 1 hour. Water was added and the mixture was extracted with dichloromethane, dried (MgSO4) and filtered. The flitrate was evaporated to dryness and the residue was recrystallized from n-hexane to give 2-(phenylsulphenyl)-4-trifluoromethylbenzonitrile (9.5 g) as a white solid, m.p. 51° C.

Quelle