反应详情

温度

45 °C

38 g of potassium hydroxide was dissolved in 800 ml of methanol and then 100 g of 2-mercaptocycloheptimidazole was added thereto and stirred under heating at an internal temperature of about 45° C. Next, 131.2 g of dimethylsulfuric acid was dropwise added and further stirred under heating at an internal temperature of about 45° C. for 1 hour. After the solvent was evaporated off to some degree under reduced pressure, one liter of water was added, and the resulting solution was extracted with chloroform (0.5 liter×2). Then, the chloroform layer was dried with anhydrous sodium sulfate, and the solvent was evaporated off under reduced pressure until the chloroform solution became 200 ml. Next, one liter of hexane was added to the thus concentrated solution whereby a precipitate crystallized out. This was separated by filtration and dried. 89 g of colorless crystals was obtained.

1. stirringfurther stirred
2. temperatureunder heating at an internal temperature of about 45° C. for 1 hour
3. customAfter the solvent was evaporated off to some degree under reduced pressure, one liter of water
4. additionwas added
5. extractionthe resulting solution was extracted with chloroform (0.5 liter×2)
6. dry with materialThen, the chloroform layer was dried with anhydrous sodium sulfate
7. customthe solvent was evaporated off under reduced pressure until the chloroform solution
8. additionNext, one liter of hexane was added to the thus concentrated solution whereby a precipitate
9. customcrystallized out
10. customThis was separated by filtration
11. customdried