Pyridine → 2-Cyano-4,4'-dinitrobenzanilide

HRID 461213

反応式

HRID 461213 の反応式
[N+:1]([C:4]1[CH:11]=[C:8](C#N)[C:7]([NH2:12])=[CH:6][CH:5]=1)([O-:3])=[O:2].[N+:13]([C:16]1[CH:24]=[CH:23][C:19]([C:20](Cl)=[O:21])=[CH:18][CH:17]=1)([O-:15])=[O:14].[N:25]1C=CC=C[CH:26]=1>>[C:26]([C:23]1[CH:24]=[C:16]([N+:13]([O-:15])=[O:14])[CH:17]=[CH:18][C:19]=1[C:20]([NH:12][C:7]1[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:11][CH:8]=1)=[O:21])#[N:25]

参加物

4

反応物 3

HCID 1049PyridineHCID 85024-Nitrobenzoyl chlorideHCID 285322-Amino-5-nitrobenzonitrile

生成物 1

HCID 196897482-Cyano-4,4'-dinitrobenzanilide

実験手順

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°.

後処理

  1. temperatureThe reaction mixture is refluxed for 3 hours
  2. distillationThe pyridine is distilled in vacuo
  3. additionThe oily residue is poured into 600 ml
  4. distillationof water and is distilled in vacuo
  5. additionThe oily residue is poured into 600 ml
  6. customof water and the precipitate removed by filtration
  7. customThe insoluble material is removed by filtration
  8. customThere is obtained 21.57 gm

出典と根拠

ORDレコード
ord-9bb7520d73ab4a81afcf39c912f25f30
出典データセット
uspto-grants-1977_12
特許番号
US04061791

関連ノート

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