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1,2-Dichloro-4-nitrobenzene → (2-Chloro-4-nitrophenyl)hydrazine

HRID 1709957
ノート
印刷プレビュー

反応式

HRID 1709957 の反応式
O.[NH2:2][NH2:3].Cl[C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:6]=1[Cl:14]>C(#N)C>[Cl:14][C:6]1[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=1[NH:2][NH2:3]
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 74431,2-Dichloro-4-nitrobenzeneHCID 24654Hydrazine hydrate (1:1)

生成物 1

HCID 5029294(2-Chloro-4-nitrophenyl)hydrazine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

59 g of hydrazine hydrate was dissolved in 712 ml of acetonitrile at room temperature under an atmosphere of nitrogen. A solution obtained by dissolving 46.3 g of 1,2-dichloro-4-nitrobenzene in 71 g of acetonitrile was added dropwisely to the obtained solution. After the addition had been completed, the obtained mixture was subjected to reflux by heat for 4 hours, and the reaction solution was concentrated. 500 g of water was added to the concentrate, and the produced crystals were filtered off. 200 g of acetonitrile was then added to the crystals, and the obtained mixture was subjected to reflux by heat for 30 minutes and then cooled with ice to room temperature. The produced crystals were filtered off (yield: 27 g).

後処理

  1. customA solution obtained
  2. additionwas added dropwisely to the obtained solution
  3. additionAfter the addition
  4. temperatureto reflux
  5. temperatureby heat for 4 hours
  6. concentrationthe reaction solution was concentrated
  7. addition500 g of water was added to the concentrate
  8. filtrationthe produced crystals were filtered off
  9. addition200 g of acetonitrile was then added to the crystals
  10. temperatureto reflux
  11. temperatureby heat for 30 minutes
  12. filtrationThe produced crystals were filtered off (yield: 27 g)

出典と根拠

ORDレコード
ord-000c12f206384d0789810578f08a4c4a
出典データセット
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04952483

反応ノート

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