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

HRID 918042ノート

反応式

HRID 918042 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-55756baa408e4d72b2cff268dee583fb
出典データセット
uspto-grants-1976_07
特許番号
US03969354

反応ノート

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