반응 #49958

반응 방정식

2,5-dichloro-nitrobenzene

potassium

salicylaldehyde

→

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

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   기타an exothermic reaction
3. 3
   기타rose to about 195° C
4. 4
   온도Heating
5. 5
   온도The mixture was cooled
6. 6
   추출it was extracted with ether
7. 7
   여과The ether layer was filtered
8. 8
   기타to remove insoluble material
9. 9
   건조the resultant solution was dried over sodium sulfate
10. 10
    기타The ether solvent was evaporated
11. 11
    기타the residual oil was re crystallized from a mixture of hexane and benzene

실험 절차

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.

출처