Reaktion #49958

Reaktionsgleichung

2,5-dichloro-nitrobenzene

potassium

salicylaldehyde

→

2-(2-nitro-4-chloro-phenoxy)benzaldehyde

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the addition
2. 2
   Sonstigean exothermic reaction
3. 3
   Sonstigerose to about 195° C
4. 4
   TemperaturHeating
5. 5
   TemperaturThe mixture was cooled
6. 6
   Extraktionit was extracted with ether
7. 7
   FiltrationThe ether layer was filtered
8. 8
   Sonstigeto remove insoluble material
9. 9
   Trocknenthe resultant solution was dried over sodium sulfate
10. 10
    SonstigeThe ether solvent was evaporated
11. 11
    Sonstigethe residual oil was re crystallized from a mixture of hexane and benzene

Vorschrift

Briefly, 200 parts of 2,5-dichloro-nitrobenzene were heated to 160° C. and stirred, and 160 parts of the potassium salt of salicylaldehyde was added over a period of 30 minutes. After the addition was complete, an exothermic reaction took place, and the temperature rose to about 195° C. Heating was discontinued until the reaction subsided, and the mixture was heated for 1 hour at 150° C. The mixture was cooled, ice and water were added, and it was extracted with ether. The ether layer was filtered to remove insoluble material, and the resultant solution was dried over sodium sulfate. The ether solvent was evaporated, and the residual oil was re crystallized from a mixture of hexane and benzene to give 2-(2-nitro-4-chloro-phenoxy)benzaldehyde melting at about 100°-101° C.

Quelle