反应详情

A mixture of 540 mg of 3-aminopyrazole-4-carbonitrile, 1.23 g of N-[3-[3-(dimethylamino)-1-oxo-2-propenyl]phenyl]-N-methylacetamide and 50 ml of glacial acetic acid was heated at reflux for 8 hours then the solvent was removed: The residue was partitioned between saturated aqueous sodium bicarbonate and dichloromethane. The organic layer was separated, dried, passed through a pad of hydrous magnesium silicate and hexane was added to the refluxing filtrate to crystallize the product. The mixture was cooled and the solid collected, giving the desired product, mp 195°-197° C.

1. temperaturewas heated
2. temperatureat reflux for 8 hours
3. customthe solvent was removed
4. customThe residue was partitioned between saturated aqueous sodium bicarbonate and dichloromethane
5. customThe organic layer was separated
6. customdried
7. additionwas added to the refluxing filtrate
8. customto crystallize the product
9. temperatureThe mixture was cooled
10. customthe solid collected