反应详情

温度

25 °C

To the solution of 2-amino-4′-fluorobenzophenone (100 g) in methanol (500 ml) added Methyl 3-cyclopropyl-3-oxopropanoate (132 g), sulfuric acid (5 ml) and stirred for 15 minutes at 25° C. Heated the reaction mixture to 65° C. for 22 hrs. Distilled off the methanol completely under reduced pressure. Cooled the reaction mixture to 25° C., added water (500 ml) and stirred for 30 minutes. Cooled the reaction mixture to 0° C. and pH adjusted to 6.0 with sodium carbonate solution. Stirred the reaction mixture for 45 minutes at 25° C. Filtered the cake and washed with water. Spin dry the compound for 60 minutes. To this compound added methanol (150 ml) and stirred for 1 hr at 25° C. Filtered the solid and washed with methanol (50 ml). Dried the obtained solid to get the title compound.

1. temperatureHeated the reaction mixture to 65° C. for 22 hrs
2. distillationDistilled off the methanol completely under reduced pressure
3. temperatureCooled the reaction mixture to 25° C.
4. additionadded water (500 ml)
5. stirringstirred for 30 minutes
6. temperatureCooled the reaction mixture to 0° C.
7. stirringStirred the reaction mixture for 45 minutes at 25° C
8. filtrationFiltered the cake
9. washwashed with water
10. customSpin dry the compound for 60 minutes
11. additionTo this compound added methanol (150 ml)
12. stirringstirred for 1 hr at 25° C
13. filtrationFiltered the solid
14. washwashed with methanol (50 ml)
15. customDried the obtained solid