反应详情

A mixture of 2.54 g of 3-amino-1,2,4-triazole, 5.29 g of 3-dimethylamino-1-(3-pyridyl)-2-propene-1-one and 25 ml of glacial acetic acid was heated under reflux for 6 hours. The solvent was removed in vacuo and the solid residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane. The organic layer was separated and dried over powdered anhydrous sodium sulfate. This solution was passed through a short column of a hydrous magnesium silicate and the effluent was refluxed on a steam bath with the gradual addition of hexane until crystallization was noted. On cooling the desired compound was separated and collection by filtration gave 1.95 g. of colorless crystals mp. 209°-210° C.

1. temperaturewas heated
2. temperatureunder reflux for 6 hours
3. customThe solvent was removed in vacuo
4. customthe solid residue was partitioned between a saturated aqueous sodium bicarbonate solution and dichloromethane
5. customThe organic layer was separated
6. customdried
7. temperaturethe effluent was refluxed on a steam bath with the gradual addition of hexane until crystallization
8. temperatureOn cooling the desired compound
9. customwas separated
10. customcollection
11. filtrationby filtration
12. customgave 1.95 g