反应详情

温度

50 °C

Sodium metal (1.21 g) was dissolved in anhydrous ethanol (50 ml) followed by addition of N-methylthiourea (4.96 g), and the mixture was stirred for dissolution at 50° C. for 30 minutes. Then, a solution of ethyl 2-cyano-4,4-diethoxybutyrate (11.47 g) in ethanol (10 ml) was added and the mixture was refluxed at 100° C. for 5 hours. The solvent was then distilled off under reduced pressure and the residue was-dissolved by adding water (20 ml). Then, 10% hydrochloric acid (75 ml) was added and the mixture was stirred overnight. The resulting precipitate was collected by filtration, washed serially with water, ethanol and ether, and dried to provide the title compound (6.8 g). 1H-NMR (DMSO-d6) δ: 3.82(3H,s), 6.41-6.44(1H,m), 6.92-6.95(1H,s), 12.02(1H,s), 12.06(1H,s).

1. temperaturethe mixture was refluxed at 100° C. for 5 hours
2. distillationThe solvent was then distilled off under reduced pressure
3. dissolutionthe residue was-dissolved
4. additionby adding water (20 ml)
5. additionThen, 10% hydrochloric acid (75 ml) was added
6. stirringthe mixture was stirred overnight
7. filtrationThe resulting precipitate was collected by filtration
8. washwashed serially with water, ethanol and ether
9. customdried