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Methylhydrazine → HCID 19025427、化合物

HRID 1030970
ノート
印刷プレビュー

反応式

HRID 1030970 の反応式
[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]
参加物反応条件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 6061MethylhydrazineHCID 27577362-chloro-1-isothiocyanato-4-nitrobenzene

生成物 1

HCID 19025427HCID 19025427、化合物収率 80.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
65 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e0800a43804c4bc9a5f3dc7c01df1a49
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05108486

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート