HRID3244

反应详情

EQUATION

反应方程式

HRID 3244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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%.

WORKUP

后处理

  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)