5,5-Dimethyl-2,4-imidazolidinedithione → 2,4-bis(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole

HRID 3244

反応式

HRID 3244 の反応式
Cl.[CH3:2][N:3]([CH3:12])[C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6]Cl.[CH3:13][C:14]1([CH3:21])[NH:18][C:17](=[S:19])[NH:16][C:15]1=[S:20]>CCO>[CH3:2][N:3]([CH3:12])[C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6][S:19][C:17]1[N:16]=[C:15]([S:20][CH2:6][C:5]2[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]([CH3:12])[CH3:2])[C:14]([CH3:21])([CH3:13])[N:18]=1

参加物

4

反応物 2

HCID 30021425,5-Dimethyl-2,4-imidazolidinedithioneHCID 135374262-(chloromethyl)-N,N-dimethylaniline hydrochloride

生成物 1

HCID 189348482,4-bis(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Initially, a solution of 9.1 g of 2-dimethylaminobenzylchloride hydrochloride in 50 mL of EtOH was added to a solution of 7 g of 5,5-dimethyl-2,4-dithiohydantoin in 100 mL of ethanol (EtOH). The reaction mixture was stirred for 1.5 hour at the room temperature and concentrated in vacuo. To the residue, there was added 100 mL of chloroform (CHCl3). The residue was then washed with an aqueous solution of potassium carbonate (CaCO3), dried over magnesium sulfate (MgSO4), and concentrated in vacuo. The residue was chromatographed on a column of silica gel (CHCl3). From the earlier fractions, 2,4-bis(2-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole was isolated as a syrup. The yield of this compound was 1.1 g with a yield ratio of 5.9%.

後処理

  1. concentrationconcentrated in vacuo
  2. additionTo the residue, there was added 100 mL of chloroform (CHCl3)
  3. washThe residue was then washed with an aqueous solution of potassium carbonate (CaCO3)
  4. dry with materialdried over magnesium sulfate (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe residue was chromatographed on a column of silica gel (CHCl3)

出典と根拠

ORDレコード
ord-a4c2572338d149fc9b4505fc6cb945cf
出典データセット
uspto-grants-1998_03
特許番号
US05733922

関連ノート

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