反应详情

With reference to Journal of the American Chemical Society, vol. 76, pages 3352 and 3353 (1954), 23 g of 2-mercaptocycloheptimidazole as synthesized in Synthetic example 1 (b) was added to 210 ml of 10% nitric acid, and stirred with heating to the inner temperature of 80° to 90° C. for one hour. The reaction solution was neutralized with sodium bicarbonate and extracted with chloroform (250 ml×2). The chloroform layer was dried over anhydrous sodium sulfate and concentrated to 50 ml under reduced pressure, and then 200 ml of hexane was added. Deposited crystals were collected by filtration and dried.

1. temperaturewith heating to the inner temperature of 80° to 90° C. for one hour
2. extractionextracted with chloroform (250 ml×2)
3. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated to 50 ml under reduced pressure
5. addition200 ml of hexane was added
6. filtrationDeposited crystals were collected by filtration
7. customdried