反应详情

温度

45 °C

First, 38 g of potassium hydroxide was dissolved in 800 ml of methanol, 100 g of 2-mercaptocycloheptimidazole was added thereto, 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 to some extent under reduced pressure, 1 l of water was added and extracted with chloroform (0.5 l×2). After being dried over anhydrous sodium sulfate, the chloroform layer was evaporated under reduced pressure to 200 ml, and 1 l of hexane was added thereto to deposite crystals, which were the filtered and dried.

1. stirringstirred
2. temperaturewith heating to the inner temperature of about 45° C. for one hour
3. distillationAfter the solvent was distilled away to some extent under reduced pressure, 1 l of water
4. additionwas added
5. extractionextracted with chloroform (0.5 l×2)
6. dry with materialAfter being dried over anhydrous sodium sulfate
7. customthe chloroform layer was evaporated under reduced pressure to 200 ml, and 1 l of hexane
8. additionwas added
9. filtrationfiltered
10. customdried