反应详情

A mixture of 4,6-diaminoquinazoline hydrochloride (10 g) and tripropylamine (26.4 g) in dry pyridine (100 ml) was stirred in an ice-bath for 20 minutes. To the mixture was added dropwise during 1.5 hours 3-cyclopentylpropionyl chloride (12.2 g). The mixture was stirred in an ice-bath for 1.5 hours. Crushed ice was added to the reaction mixture. The mixture was stirred for 5 minutes and concentrated under reduced pressure. After addition of water, sodium hydrogen carbonate was added in small portions to the mixture to give precipitates which were separated by filtration, washed with water and dried. The crude crystals were dissolved in a mixture of chloroform and methanol under heating. After the filtration of insoluble materials, the filtrate was treated with activated charcoal and concentrated under reduced pressure to give a residue. The residue was suspended in ethyl acetate. The suspension was stirred for 1 hour under heating and filtered to give crystalline 4-amino-6-(3-cyclopentylpropionamido)quinazoline (7.2 g).

1. stirringThe mixture was stirred in an ice-bath for 1.5 hours
2. additionCrushed ice was added to the reaction mixture
3. stirringThe mixture was stirred for 5 minutes
4. concentrationconcentrated under reduced pressure
5. additionAfter addition of water, sodium hydrogen carbonate
6. additionwas added in small portions to the mixture
7. customto give
8. customprecipitates which
9. customwere separated by filtration
10. washwashed with water
11. customdried
12. dissolutionThe crude crystals were dissolved in a mixture of chloroform and methanol
13. temperatureunder heating
14. filtrationAfter the filtration of insoluble materials
15. additionthe filtrate was treated with activated charcoal
16. concentrationconcentrated under reduced pressure
17. customto give a residue
18. stirringThe suspension was stirred for 1 hour
19. temperatureunder heating
20. filtrationfiltered