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

HRID 1709957
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HRID 1709957 반응식
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]
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참가 물질

4

반응물 2

HCID 74431,2-Dichloro-4-nitrobenzeneHCID 24654Hydrazine hydrate (1:1)

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-000c12f206384d0789810578f08a4c4a
출처 데이터셋
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04952483

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