تفاعل #3340

معادلة التفاعل

2-dimethylaminobenzylchloride hydrochloride

5,5-dimethyl-2,4-dithiohydantoin

→

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

المذيبات

EtOH

ethanol

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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%.

المصدر