反应详情

To a mixture of 4,6-diaminoquinazoline hydrochloride (10.0 g), tripropylamine (17.61 g) and dry pyridine (100 ml) was added dropwise during 35 minutes 3,3-dimethylbutyryl chloride (10.34 g) under ice-cooling. The reaction mixture was stirred for 2 hours at the same temperature. To the resultant mixture was added ice-water. The mixture was stirred for 5 minutes and then concentrated under reduced pressure. To the residue was added water and sodium hydrogen carbonate (13.0 g) little by little to give precipitates, which were separated by filtration, washed with water and dried. Thus obtained crude crystals were dissolved in a mixture of chloroform and methanol under heating. After insoluble materials were removed by filtration, the filtrate was concentrated under reduced pressure to give a residue, which was suspended in 5% methanol-chloroform solution (70 ml). After stirring under heating, the suspension was filtered to give crystalline 4-amino-6-(3,3-dimethylbutyramido)quinazoline (8.5 g).

1. temperaturecooling
2. stirringThe mixture was stirred for 5 minutes
3. concentrationconcentrated under reduced pressure
4. additionTo the residue was added water and sodium hydrogen carbonate (13.0 g) little by little
5. customto give
6. customprecipitates
7. customwhich were separated by filtration
8. washwashed with water
9. customdried
10. customThus obtained crude crystals
11. temperatureunder heating
12. customAfter insoluble materials were removed by filtration
13. concentrationthe filtrate was concentrated under reduced pressure
14. customto give a residue, which
15. stirringAfter stirring
16. temperatureunder heating
17. filtrationthe suspension was filtered