反应详情

温度

45 °C

A mixture of ethyl 3-oxohexanoate (20.0 g) and 1,1-dimethoxy-N,N-dimethylmethanamine (15.8 g) in ethanol (40 mL) was stirred at 40 to 50° C. for 3 hours. After cooling to 25° C., ethyl cyanoacetate (15.7 g) was added to the mixture followed by addition of N-ethyl-N-isopropylpropan-2-amine (22.1 mL) at room temperature. The mixture was stirred at 50° C. for 16 hours. Acetic acid (9.11 g) and ethanol (40 mL) were added to the mixture at room temperature. The mixture was warmed to 50° C., and water (100 mL) was charged. The suspension was cooled to room temperature and stirred for 30 minutes. The precipitate was collected by filtration, washed with ethanol-water (20 mL-80 mL) and dried at 70° C. under vacuum to give a white solid. This solid was dissolved in ethanol (200 mL) at reflux temperature. Water (150 mL) was added to the mixture at the same temperature. The mixture was cooled gradually, stirred at 50 to 60° C. for 1 hour and at room temperature for 2 hours. The precipitate was collected by filtration, washed with ethanol-water (25 mL-25 mL) and dried at 70° C. under vacuum to give the title compound (17.5 g).

1. temperatureAfter cooling to 25° C.
2. stirringThe mixture was stirred at 50° C. for 16 hours
3. temperatureThe mixture was warmed to 50° C.
4. temperatureThe suspension was cooled to room temperature
5. stirringstirred for 30 minutes
6. filtrationThe precipitate was collected by filtration
7. washwashed with ethanol-water (20 mL-80 mL)
8. customdried at 70° C. under vacuum
9. customto give a white solid
10. temperatureat reflux temperature
11. temperatureThe mixture was cooled gradually
12. stirringstirred at 50 to 60° C. for 1 hour and at room temperature for 2 hours
13. filtrationThe precipitate was collected by filtration
14. washwashed with ethanol-water (25 mL-25 mL)
15. customdried at 70° C. under vacuum