反应详情

温度

190 °C

Charged 300.0 g of formamide into a 2.0 L 4 necked round bottom flask connected to a mechanical stirrer, thermo meter socket, and condenser under nitrogen atmosphere. 90.0 g (0.39 mol) of 5-Amino-1-(3,5-dimethyl-phenyl)-1H-pyrazole-4-carboxylic acid amide (Compound No. 77) was charged. Reaction mass temperature was raised to reflux (185-195° C.). Maintained the mass temperature at reflux for 60-90 min. Reaction mass temperature was cooled to 140-150° C. 900.0 ml of water was added slowly at maintaining the mass temperature 80-150° C. Maintained the mass temperature at 80-90° C. for 45-60 min. Reaction mass temperature was cooled to 25-30° C. Maintained the mass temperature at 25-30° C. for 90-120 min. Solid was filtered and solid was washed with 150.0 ml of water. 500.0 ml of DM Water and wet crude compound were charged into a 2.0 L 4 necked round bottom flask connected to a mechanical stirrer, thermo meter socket, and condenser. Mass temperature was raised to reflux. Maintained the mass temperature at reflux for 75-90 min and mass temperature was cooled to 25-30° C. Maintained the mass temperature at 25-30° C. for 90-120 min. Solid was filtered and solid was washed with 100.0 ml of water. Compound was dried under vacuum at 60-65° C. Dry weight of the compound: 65.0 g (yield 69.21%)

1. customconnected to a mechanical stirrer
2. addition77) was charged
3. customReaction mass temperature
4. temperaturewas raised
5. temperatureMaintained the mass temperature
6. temperatureat reflux for 60-90 min
7. customReaction mass temperature
8. temperaturewas cooled to 140-150° C
9. temperatureat maintaining the mass temperature 80-150° C
10. temperatureMaintained the mass temperature at 80-90° C. for 45-60 min
11. customReaction mass temperature
12. temperaturewas cooled to 25-30° C
13. temperatureMaintained the mass temperature at 25-30° C. for 90-120 min
14. filtrationSolid was filtered
15. washsolid was washed with 150.0 ml of water
16. addition500.0 ml of DM Water and wet crude compound were charged into a 2.0 L 4 necked round bottom flask
17. customconnected to a mechanical stirrer
18. temperatureMass temperature was raised
19. temperatureto reflux
20. temperatureMaintained the mass temperature
21. temperatureat reflux for 75-90 min
22. temperaturemass temperature was cooled to 25-30° C
23. temperatureMaintained the mass temperature at 25-30° C. for 90-120 min
24. filtrationSolid was filtered
25. washsolid was washed with 100.0 ml of water
26. customCompound was dried under vacuum at 60-65° C
27. customDry weight of the compound