反应详情

温度

70 °C

2-Cyanoacetamide (4.31 g) and 3-(dimethylamino)-1-(4-fluorophenyl)prop-2-en-1-one (9.00 g) were added in this order to a mixture of sodium hydride (60% oil, 4.10 g) and DMF (90 mL), and the resultant mixture was stirred at 105° C. for 2 hours. The solvent was distilled off. Water was added to the obtained residue, and then, the mixture was rendered acidic by the addition of acetic acid and stirred at 70° C. for 15 minutes. Methanol was added to the reaction mixture for suspension, and the deposited solid was washed with ethyl acetate to obtain the title compound (9.98 g).

1. distillationThe solvent was distilled off
2. additionWater was added to the obtained residue
3. additionthe mixture was rendered acidic by the addition of acetic acid
4. additionMethanol was added to the reaction mixture for suspension
5. washthe deposited solid was washed with ethyl acetate