반응 #548395

반응 방정식

5-nitroanthranilonitrile

p-nitrobenzoyl chloride

pyridine

→

2-Cyano-4,4'-dinitrobenzanilide

반응 조건

후처리

1. 1
   온도The reaction mixture is refluxed for 3 hours
2. 2
   workup.DISTILLATIONThe pyridine is distilled in vacuo
3. 3
   workup.ADDITIONThe oily residue is poured into 600 ml
4. 4
   workup.DISTILLATIONof water and is distilled in vacuo
5. 5
   workup.ADDITIONThe oily residue is poured into 600 ml
6. 6
   기타of water and the precipitate removed by filtration
7. 7
   기타The insoluble material is removed by filtration
8. 8
   기타There is obtained 21.57 gm

실험 절차

To a stirred solution of 16.3 gm. (0.1 mole) of 5-nitroanthranilonitrile in 100 ml. of dry pyridine is added 18.56 gm. (0.1 mole) of p-nitrobenzoyl chloride. The reaction mixture is refluxed for 3 hours. The pyridine is distilled in vacuo. The oily residue is poured into 600 ml. of water and is distilled in vacuo. The oily residue is poured into 600 ml. of water and the precipitate removed by filtration. The precipitate is boiled with 1500 ml. of ethanol. The insoluble material is removed by filtration. There is obtained 21.57 gm. of yellow solid that melts at 195°-196°.

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