反应详情

温度

106.5 °C

650.0 g of Phosphorus (V) oxychloride (POCl3) was charged into a 2.0 L 4 necked round bottom flask connected to a mechanical stirrer, thermo meter socket, and condenser under nitrogen atmosphere. 60.0 g (0.25 mol) of 1-(3,5-Dimethyl-phenyl)-1,5-dihydro-pyrazolo[3,4-d]pyrimidine-4-one (Compound No. 78) was charged. Reaction mass temperature was raised to reflux (105-108° C.). Maintained the mass temperature at reflux for 8-9 hour's. Reaction mass temperature was cooled to 25-30° C. and 600.0 ml of chloroform was charged. Maintained the mass temperature at 25-30° C. for 30-45 min. 2.0 kg's of crushed ice was charged into a 5.0 L 4 necked round bottom flask connect to a mechanical stirrer, thermo meter socket, and condenser. Reaction mass was added slowly at maintaining the mass temperature below 10° C. Maintained the mass temperature at 0-10° C. for 30-45 min. Mass temperature was raised to 25-30° C. 600.0 ml of Chloroform was charged. Maintained the mass temperature at 25-30° C. for 30-45 min and settled the mass for 20-30 min. Separated the bottom organic layer. Organic layer was dried with sodium sulphate upto obtaining the moisture content is not more than 0.20% w/v. 15.0 g of carbon was charged. Mass temperature was raised to 45-50° C. Maintained the mass temperature at 45-50° C. for 30-45 min. Carbon and sodium sulphate was filtered through hyflow bed and bed was washed with 300.0 ml of chloroform. Filtrate was collected into a flask. Chloroform was distilled completely under vacuum at mass temperature not crossing 60° C. Finally applied high vacuum to complete remove the traces of chloroform at mass temperature not crossing 60° C. Mass temperature was cooled to 25-30° C. and release the vacuum. 250.0 ml of isopropyl ether was charged. Maintained the mass temperature at 25-30° C. for 45-60 min. Solid was filtered and the solid was washed with 50.0 ml of isopropyl ether. Compound was dried under vacuum at 55-60° C. Dry weight of the compound: 56.0 g (yield 86.6%).

1. customconnected to a mechanical stirrer
2. addition78) was charged
3. customReaction mass temperature
4. temperaturewas raised
5. temperatureMaintained the mass temperature
6. temperatureat reflux for 8-9 hour's
7. customReaction mass temperature
8. temperaturewas cooled to 25-30° C.
9. temperatureMaintained the mass temperature at 25-30° C. for 30-45 min
10. customconnect to a mechanical stirrer
11. customReaction mass
12. additionwas added slowly
13. temperatureat maintaining the mass temperature below 10° C
14. temperatureMaintained the mass temperature at 0-10° C. for 30-45 min
15. temperatureMass temperature was raised to 25-30° C
16. temperatureMaintained the mass temperature at 25-30° C. for 30-45 min
17. customfor 20-30 min
18. customSeparated the bottom organic layer
19. dry with materialOrganic layer was dried with sodium sulphate
20. customupto obtaining the moisture content
21. addition15.0 g of carbon was charged
22. temperatureMass temperature was raised to 45-50° C
23. temperatureMaintained the mass temperature at 45-50° C. for 30-45 min
24. filtrationCarbon and sodium sulphate was filtered through hyflow bed and bed
25. washwas washed with 300.0 ml of chloroform
26. customFiltrate was collected into a flask
27. distillationChloroform was distilled completely under vacuum at mass temperature not
28. customcrossing 60° C
29. customFinally applied high vacuum to complete remove the traces of chloroform at mass temperature not
30. customcrossing 60° C
31. temperatureMass temperature was cooled to 25-30° C.
32. addition250.0 ml of isopropyl ether was charged
33. temperatureMaintained the mass temperature at 25-30° C. for 45-60 min
34. filtrationSolid was filtered
35. washthe solid was washed with 50.0 ml of isopropyl ether
36. customCompound was dried under vacuum at 55-60° C
37. customDry weight of the compound