反应详情

In accordance with the method described in Journal of the Americal Chemical Society, Vol. 76, pages 3352 and 3353 (1954), 23 g of 2-mercaptocycloheptimidazole, as obtained in Example 1-(b), was added to 210 ml of 10% nitric acid and everything was stirred under heating at an internal temperature of from 80° to 90° C. for 1 hour. Sodium hydrogencarbonate was added to the reaction solution so as to neutralize the solution, and this was extracted with chloroform (250 ml×2). The chloroform layer was dried with anhydrous sodium sulfate, and then the solvent was evaporated off until the amount of the chloroform solution became 50 ml. Next, 200 ml of hexane was added thereto. The crystals precipitated were separated by filtration and dried.

1. temperatureunder heating at an internal temperature of from 80° to 90° C. for 1 hour
2. extractionthis was extracted with chloroform (250 ml×2)
3. dry with materialThe chloroform layer was dried with anhydrous sodium sulfate
4. customthe solvent was evaporated off until the amount of the chloroform solution
5. additionNext, 200 ml of hexane was added
6. customThe crystals precipitated
7. customwere separated by filtration
8. customdried