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Methylhydrazine → HCID 19025427, 화합물

HRID 1030970
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HRID 1030970 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[N:11]=[C:12]=[S:13].[CH3:14][NH:15][NH2:16]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[NH:11][C:12](=[S:13])[N:15]([CH3:14])[NH2:16]
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참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 27577362-chloro-1-isothiocyanato-4-nitrobenzene

생성물 1

HCID 19025427HCID 19025427, 화합물수율 80.8%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
65 °C

실험 절차

To a stirred solution of 60.0 g (0.280 mole) of 2-chloro-4-nitrophenyl isothiocyanate in 500 ml of ethanol was added 12.9 g (0.280 mole) of methylhydrazine. This mixture was heated and was stirred at 65° C. for approximately 18 hours. The mixture was then heated to reflux and was cooled. A solid had formed and was collected by filtration. The filter cake was rinsed with aqueous ethanol and was dried under reduced pressure to yield 59.0 g of 4-(2-chloro-4-nitrophenyl)-2-methyl-3-thiosemicarbazide, mp 164°-167° C. The nmr spectrum was consistent with the proposed structure.

후처리

  1. temperatureThis mixture was heated
  2. temperatureThe mixture was then heated
  3. temperatureto reflux
  4. temperaturewas cooled
  5. customA solid had formed
  6. filtrationwas collected by filtration
  7. washThe filter cake was rinsed with aqueous ethanol
  8. customwas dried under reduced pressure

출처 및 근거

ORD 기록
ord-e0800a43804c4bc9a5f3dc7c01df1a49
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05108486

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