Benzenesulfenyl chloride → 1-Methyl-2-[nitro(phenylsulfanyl)methylidene]imidazolidine

HRID 1414900ノート

反応式

HRID 1414900 の反応式
[C:1]1([S:7]Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:9][N:10]1[CH2:14][CH2:13][NH:12][C:11]1=[CH:15][N+:16]([O-:18])=[O:17]>N1C=CC=CC=1>[CH3:9][N:10]1[CH2:14][CH2:13][NH:12][C:11]1=[C:15]([N+:16]([O-:18])=[O:17])[S:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 11008040Benzenesulfenyl chlorideHCID 702500461-Methyl-2-(nitromethylidene)imidazolidine

生成物 1

HCID 706390091-Methyl-2-[nitro(phenylsulfanyl)methylidene]imidazolidine

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

14.6 g of phenylsulfenyl chloride was added dropwise to a cooled, stirred solution of 14.3 g of Compound 1 in 250 ml of pyridine. The mixture was allowed to stand overnight at room temperature, then excess pyridine was recovered on a rotary evaporator. The residue was treated with 250 ml of water and the mixture extracted with methylene chloride. The combined extracts were dried and the solvent evaporated to give a crystalline solid which was triturated with ethyl acetate, then ethanol, to yield 25, as a yellow solid, melting point: 170° - 173° .

後処理

  1. customexcess pyridine was recovered on a rotary evaporator
  2. additionThe residue was treated with 250 ml of water
  3. extractionthe mixture extracted with methylene chloride
  4. customThe combined extracts were dried
  5. customthe solvent evaporated
  6. customto give a crystalline solid which
  7. customwas triturated with ethyl acetate

出典と根拠

ORDレコード
ord-6ec74eb61a49444abd3837a5cfc7df99
出典データセット
uspto-grants-1977_01
特許番号
US04002765

反応ノート

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