反应详情

A reaction mixture of 1.87 g of (3-amino-1H-pyrazol-4-yl)phenyl-methanone and 2.43 g of 3-dimethylamino-1-[3-(trifluoromethyl)phenyl]-2-propen-1-one in 25 ml of glacial acetic acid was refluxed for 6 hours and then the solvent was removed in vacuo giving a crystalline residue. This residue was partitioned between saturated aqueous sodium bicarbonate and dichloromethane. The organic layer was dried with anhydrous sodium sulfate and then passed through a short pad of hydrous magnesium silicate. The addition of hexane to the refluxing eluate induced crystallization. After cooling, the desired product was collected as crystals, mp 148°-150° C.

1. temperaturewas refluxed for 6 hours
2. customthe solvent was removed in vacuo
3. customgiving a crystalline residue
4. customThis residue was partitioned between saturated aqueous sodium bicarbonate and dichloromethane
5. dry with materialThe organic layer was dried with anhydrous sodium sulfate
6. additionThe addition of hexane
7. customto the refluxing eluate induced crystallization
8. temperatureAfter cooling
9. customthe desired product was collected as crystals, mp 148°-150° C.