Dimethyl Sulfate → 6-Methyl-2-(methylsulfanyl)cyclohepta[d]imidazole

Participants

Reaction Conditions

Reaction Steps

First, 38 g of potassium hydroxide was dissolved in 800 ml of methanol, 108.5 g of 2-mercapto-6-methylcycloheptimidazole was added, and the mixture was stirred with heating to the inner temperature of about 45° C. Then, 131.2 g of dimethyl sulfate was added dropwise thereto and stirred with heating to the inner temperature of about 45° C. for one hour. After the solvent was distilled away in some extent under reduced pressure, 1 l of water was added and extracted with chloroform (0.5 l×2). The chloroform layer was dried over anhydrous sodium sulfate and evaporated to 200 ml under reduced pressure to distil away the solvent. With the addition of 1 l of hexane, crystals were deposited, and they were collected by filtration and dried.

Provenance & Evidence