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4-Chloro-2-nitroaniline → HCID 10846711、化合物

HRID 1578690
ノート
印刷プレビュー

反応式

HRID 1578690 の反応式
CO[CH:3]1[CH2:7][CH2:6][CH:5](OC)O1.[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[C:13]([N+:18]([O-:20])=[O:19])[CH:12]=1>C(O)(=O)C>[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([N:15]2[CH:3]=[CH:7][CH:6]=[CH:5]2)=[C:13]([N+:18]([O-:20])=[O:19])[CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 69794-Chloro-2-nitroanilineHCID 790982,5-Dimethoxytetrahydrofuran

生成物 1

HCID 10846711HCID 10846711、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

100 g (0.75 mole) of 2,5-dimethoxytetrahydrofuran are added dropwise to a stirred solution of 86.3 g (0.5 mole) of 4-chloro-2-nitroaniline in 500 ml. of glacial acetic acid. The solution is refluxed under a nitrogen atmosphere for 30 minutes, filtered, and poured into 2500 ml. of water. The aqueous solution is extracted with chloroform. The chloroform solution is dried with anhydrous sodium sulfate and concentrated to a brown oil. The brown oil is dissolved in an ether-petroleum ether-mixture and placed in a refrigerator overnight. An orange solid precipitates and is recrystallized from an ether petroleum ether mixture to give 1-(4-chloro-2-nitrophenyl) pyrrole, m.p. 55°-56° C.

後処理

  1. temperatureThe solution is refluxed under a nitrogen atmosphere for 30 minutes
  2. filtrationfiltered
  3. additionpoured into 2500 ml
  4. extractionThe aqueous solution is extracted with chloroform
  5. dry with materialThe chloroform solution is dried with anhydrous sodium sulfate
  6. concentrationconcentrated to a brown oil
  7. dissolutionThe brown oil is dissolved in an ether-petroleum ether-mixture
  8. customplaced in a refrigerator overnight
  9. customAn orange solid precipitates
  10. customis recrystallized from an ether petroleum ether mixture

出典と根拠

ORDレコード
ord-491cab11651046f7aa76d2fcd23eeb2d
出典データセット
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03939159

反応ノート

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