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

HRID 3247

반응식

HRID 3247 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-483dd6c046dd4bfda158d9c42f0f2afc
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733922

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