Reaktion #723548

Reaktionsgleichung

charcoal

1,2,3-trichloro-4-nitrobenzene

copper cyanide

hydrochloric acid

→

2,3-Dichloro-6-nitrobenzonitrile

Lösungsmittel

toluene

DMF

water

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution heated to 65° C. for 20 minutes
2. 2
   TemperaturThe mixture is cooled
3. 3
   Filtrationfiltered
4. 4
   SonstigeThe organic phase is separated
5. 5
   Extraktionthe aqueous phase extracted with toluene
6. 6
   WaschenThe combined toluene layers are washed with water and 6 N HCl
7. 7
   Sonstigedried
8. 8
   Einengenconcentrated
9. 9
   Sonstigeto give a slurry
10. 10
    FiltrationThe nitrile product is collected by filtration
11. 11
    Waschenwashed with 1.5 L cold methanol
12. 12
    Sonstigedried at 40° C.

Vorschrift

A solution of 1.831 kg of 1,2,3-trichloro-4-nitrobenzene and 0.861 kg of copper cyanide in 1.21 L of DMF is heated to 155° C. for 2 hours, then cooled to room temperature. A solution of 3.24 kg of ferric chloride hexahydrate, 0.806 L of concentrated hydrochloric acid, and 4.87 L of water is added and the solution heated to 65° C. for 20 minutes. The mixture is cooled, stirred with 0.55 kg of charcoal and 4 L of toluene, and filtered. The organic phase is separated and the aqueous phase extracted with toluene. The combined toluene layers are washed with water and 6 N HCl, dried and concentrated to give a slurry. The slurry is dissolved in 1.5 L of methanol, and stored at 5° C. for 24 hours. The nitrile product is collected by filtration, washed with 1.5 L cold methanol and dried at 40° C.

Quelle