Reaktion #3340

Reaktionsgleichung

2-dimethylaminobenzylchloride hydrochloride

5,5-dimethyl-2,4-dithiohydantoin

→

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

Lösungsmittel

EtOH

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated in vacuo
2. 2
   workup.ADDITIONTo the residue, there was added 100 mL of chloroform (CHCl3)
3. 3
   WaschenThe residue was then washed with an aqueous solution of potassium carbonate (CaCO3)
4. 4
   Trocknendried over magnesium sulfate (MgSO4)
5. 5
   Einengenconcentrated in vacuo
6. 6
   SonstigeThe residue was chromatographed on a column of silica gel (CHCl3)

Vorschrift

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%.

Quelle