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

HRID 3244

반응식

HRID 3244 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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%.

후처리

  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)

출처 및 근거

ORD 기록
ord-a4c2572338d149fc9b4505fc6cb945cf
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733922

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