反应详情

温度

100 °C

A mixture of methyl 4-oxo-10-(2,3-dimethylpentanamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate (3.4 g) and anhydrous lithium iodide (8.5 g) in dry pyridine (34 ml) was stirred at 100° C. for 1 hour and 20 minutes. The reaction mixture was concentrated under reduced pressure. Water was added to the residue to give precipitates, which were collected by filtration and washed with water. The resulting crystals were suspended in water. The suspension was adjusted to pH 1-2 with conc. hydrochloric acid to give yellow crystals, which were separated by filtration, washed with water, and dried. The crude crystals (3.85 g) were dissolved in a mixture of chloroform and methanol under heating. The solution was filtered to remove insoluble materials. The filtrate was concentrated under reduced pressure to 40 ml and cooled in an ice bath. The resulting crystals were collected by filtration and suspended in a mixture of chloroform and methanol under heating. After the suspension was cooled to ambient temperature, the crystals were filtered and dried. There was obtained 4-oxo-10-(2,3-dimethylpentanamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylic acid (1.0 g).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionWater was added to the residue
3. customto give
4. customprecipitates
5. filtrationwhich were collected by filtration
6. washwashed with water
7. customto give yellow crystals, which
8. customwere separated by filtration
9. washwashed with water
10. customdried
11. dissolutionThe crude crystals (3.85 g) were dissolved in a mixture of chloroform and methanol
12. temperatureunder heating
13. filtrationThe solution was filtered
14. customto remove insoluble materials
15. concentrationThe filtrate was concentrated under reduced pressure to 40 ml
16. temperaturecooled in an ice bath
17. filtrationThe resulting crystals were collected by filtration
18. additionsuspended in a mixture of chloroform and methanol
19. temperatureunder heating
20. temperatureAfter the suspension was cooled to ambient temperature
21. filtrationthe crystals were filtered
22. customdried