反应详情

A mixture of 4,6-diaminoquinazoline hydrochloride (1.97 g), sodium hydrogen carbonate (6.72 g) and pyridine (20 ml) was stirred under ice-cooling. To the mixture was added dropwise during 30 minutes methanesulfonyl chloride (4.58 g) under ice-cooling. The reaction mixture was stirred for an hour under ice-cooling and for 4 hours at ambient temperature. To the mixture was added ice-water. The resultant mixture was stirred for about five minutes and concentrated under reduced pressure. To the residue was added a mixture of chloroform and methanol. The mixture was stirred under heating. Insoluble materials were removed by filtration and then the filtrate was concentrated under reduced pressure to give crude crystals, to which was added a mixture of chloroform and methanol (4:1). The mixture was stirred under heating to give crystals, which were separated by filtration to give crystalline 4-amino-6-methanesulfonamidoquinazoline (1.45 g).

1. temperaturecooling
2. temperaturecooling
3. stirringThe reaction mixture was stirred for an hour under ice-
4. concentrationconcentrated under reduced pressure
5. additionTo the residue was added
6. additiona mixture of chloroform and methanol
7. stirringThe mixture was stirred
8. temperatureunder heating
9. customInsoluble materials were removed by filtration
10. concentrationthe filtrate was concentrated under reduced pressure
11. customto give crude crystals
12. additionto which was added
13. stirringThe mixture was stirred
14. temperatureunder heating
15. customto give crystals, which
16. customwere separated by filtration