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

Participants

Reaction Conditions

Reaction Steps

38 g of potassium hydroxide was dissolved in 800 ml of methanol, and 108.5 g of 2-mercapto-6-methylcycloheptimidazole was added thereto and everything was stirred under heating at an internal temperature of about 45° C. Next, 131.2 g of dimethylsulfuric acid was dropwise added and everything was further stirred under heating at an internal temperature of about 45° C. for 1 hour. After the solvent was evaporated off to some extent under reduced pressure, 1 liter of water was added and the resulting solution was extracted with chloroform (0.5 liter×2). The chloroform layer was dried with anhydrous sodium sulfate, and then the solvent was evaporated off under reduced pressure until the chloroform solution became 200 ml. To this was added one liter of hexane, whereby crystals precipitated out. The thus formed crystals were separated by filtration and dried.

Provenance & Evidence