5,5-Dimethyl-2,4-imidazolidinedithione → 2,4-bis(3-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole

HRID 3247

反応式

HRID 3247 の反応式
Cl.[CH3:2][N:3]([CH3:12])[C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH2:7]Cl.[CH3:13][C:14]1([CH3:21])[NH:18][C:17](=[S:19])[NH:16][C:15]1=[S:20].C[O-].[Na+]>CO>[CH3:2][N:3]([CH3:12])[C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[CH2:7][S:19][C:17]1[N:16]=[C:15]([S:20][CH2:7][C:6]2[CH:9]=[CH:10][CH:11]=[C:4]([N:3]([CH3:12])[CH3:2])[CH:5]=2)[C:14]([CH3:21])([CH3:13])[N:18]=1

参加物

5

反応物 3

HCID 30021425,5-Dimethyl-2,4-imidazolidinedithioneHCID 10942334Sodium MethoxideHCID 189348953-(chloromethyl)-N,N-dimethylaniline hydrochloride

生成物 1

HCID 189349022,4-bis(3-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Initially, 2.94 g of 3-dimethylaminobenzylchloride hydrochloride was added to a mixture of 1.6 g of 5,5-dimethyl-2,4-dithiohydantoin and 1.3 g of sodium methoxide in 50 mL of methanol (MeOH). The reaction mixture was stirred at the room temperature for one hour, and concentrated in vacuo. The residue was treated following the procedure used in Example 56, and chromatographed on a column of silica gel (CHCl3). From the earlier fractions, 2,4-bis(3-dimethylaminobenzylthio)-5,5-dimethyl-5H-imidazole was isolated, in the form of a syrup. The yield of this compound was 0.31 g with a yield ratio of 7.4%.

後処理

  1. concentrationconcentrated in vacuo
  2. additionThe residue was treated
  3. customchromatographed on a column of silica gel (CHCl3)

出典と根拠

ORDレコード
ord-483dd6c046dd4bfda158d9c42f0f2afc
出典データセット
uspto-grants-1998_03
特許番号
US05733922

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